Crystalline hydroxyapatite coatings synthesized under hydrothermal conditions on modified titanium substrates

Energy Technology Data Exchange (ETDEWEB)

Suchanek, Katarzyna, E-mail: Katarzyna.Suchanek@ifj.edu.pl [The Henryk Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, Radzikowskiego Street 152, 31-342 Krakow (Poland); Bartkowiak, Amanda [The Henryk Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, Radzikowskiego Street 152, 31-342 Krakow (Poland); Gdowik, Agnieszka [Faculty of Physics and Applied Computer Science, AGH University of Science and Technology, Mickiewicza 30, 30-059 Krakow (Poland); Perzanowski, Marcin [The Henryk Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, Radzikowskiego Street 152, 31-342 Krakow (Poland); Kąc, Sławomir [Faculty of Metals Engineering and Industrial Computer Science, AGH University of Science and Technology, Mickiewica 30, 30-059 Krakow (Poland); Szaraniec, Barbara [Department of Biomaterials, AGH University of Science and Technology, Mickiewicza 30, 30-059 Krakow (Poland); Suchanek, Mateusz [Department of Chemistry and Physics, University of Agriculture in Krakow, Mickiewicza 21, 31-120 Krakow (Poland); Marszałek, Marta [The Henryk Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, Radzikowskiego Street 152, 31-342 Krakow (Poland)

2015-06-01

Hydroxyapatite coatings were successfully produced on modified titanium substrates via hydrothermal synthesis in a Ca(EDTA){sup 2−} and (NH{sub 4}){sub 2}HPO{sub 4} solution. The morphology of modified titanium substrates as well as hydroxyapatite coatings was studied using scanning electron microcopy and phase identification by X-ray diffraction, and Raman and FTIR spectroscopy. The results show that the nucleation and growth of hydroxyapatite needle-like crystals with hexagonal symmetry occurred only on titanium substrates both chemically and thermally treated. No hydroxyapatite phase was detected on only acid etched Ti metal. This finding demonstrates that only a particular titanium surface treatment can effectively induce the apatite nucleation under hydrothermal conditions. - Highlights: • Bioactivation of titanium substrate by chemical and heat treatments • Precipitation of hydroxyapatite on modified titanium plates • Hydrothermal crystallization of hydroxyapatite by chelate decomposition method.

Continuous microwave flow synthesis of mesoporous hydroxyapatite

International Nuclear Information System (INIS)

Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O.; Hussain, Rafaqat

2015-01-01

We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca 2+ ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA

Continuous microwave flow synthesis of mesoporous hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini [Department of Chemistry, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Lintang, Hendrik O. [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Hussain, Rafaqat, E-mail: rafaqat@kimia.fs.utm.my [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia)

2015-11-01

We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca{sup 2+} ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA.

Synthesis and Characterization of Hydroxyapatite Powder by Wet Precipitation Method

Science.gov (United States)

Cahyaningrum, S. E.; Herdyastuty, N.; Devina, B.; Supangat, D.

2018-01-01

Hydroxyapatite is main inorganic component of the bone with formula Ca10(PO4)6(OH)2. Hydroxyapatite can be used as substituted bone biomaterial because biocompatible, non toxic, and osteoconductive. In this study, hydroxyapatite is synthesized using wet precipitation method from egg shell. The product was sintered at different temperatures of 800°C to 1000°C to improve its crystallinity. The hydroxyapatite was characterized by X-ray analysis, Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FTIR) to reveal its phase content, morphology and types of bond present within it. The analytical results showed hydroxyapatite had range in crystallinity from 85.527 to 98.753%. The analytical functional groups showed that presence of functional groups such as OH, (PO4)3 2-, and CO3 2- that indicated as hydroxyapatite. The result of characterization SEM indicated that hydroxyapatite without sintering and HAp sintering at 800 °C were irregular shape without pore. The best hydroxyapatite with temperature sintering at 900 °C showed oval shaped with pores without agglomerated.

X-ray diffraction and infrared spectroscopy analyses on the crystallinity of engineered biological hydroxyapatite for medical application

Science.gov (United States)

Poralan, G. M., Jr.; Gambe, J. E.; Alcantara, E. M.; Vequizo, R. M.

2015-06-01

Biological hydroxyapatite (BHAp) derived from thermally-treated fish bones was successfully produced. However, the obtained biological HAp was amorphous and thus making it unfavorable for medical application. Consequently, this research exploits and engineers the crystallinity of BHAp powders by addition of CaCO3 and investigates its degree of crystallinity using XRD and IR spectroscopy. On XRD, the HAp powders with [Ca]/[P] ratios 1.42, 1.46, 1.61 and 1.93 have degree of crystallinity equal to 58.08, 72.13, 85.79, 75.85% and crystal size equal to 0.67, 0.74, 0.75, 0.72 nm, respectively. The degree of crystallinity and crystal size of the obtained calcium deficient biological HAp powders increase as their [Ca]/[P] ratio approaches the stoichiometric ratio by addition of CaCO3 as source of Ca2+ ions. These results show the possibility of engineering the crystallinity and crystal size of biological HAp by addition of CaCO3. Moreover, the splitting factor of PO4 vibration matches the result with % crystallinity on XRD. Also, the area of phosphate-substitution site of PO4 vibration shows linear relationship (R2 = 0.994) with crystal size calculated from XRD. It is worth noting that the crystallinity of the biological HAp with [Ca]/[P] ratios 1.42 and 1.48 fall near the range 60-70% for highly resorbable HAp used in the medical application.

Poorly crystalline hydroxyapatite: A novel adsorbent for enhanced fulvic acid removal from aqueous solution

Energy Technology Data Exchange (ETDEWEB)

Wei, Wei [Department of Environmental Science and Engineering, Nanjing Normal University, Nanjing 210023 (China); Jiangsu Provincial Key Laboratory of Materials Cycling and Pollution Control, Nanjing Normal University, Nanjing 210023 (China); Jiangsu Center for Collaborative Innovation in Geographical Information Resource Development and Application, Nanjing Normal University, Nanjing 210023 (China); Yang, Lei; Zhong, Wenhui; Cui, Jing [Department of Environmental Science and Engineering, Nanjing Normal University, Nanjing 210023 (China); Wei, Zhenggui, E-mail: weizhenggui@gmail.com [Department of Environmental Science and Engineering, Nanjing Normal University, Nanjing 210023 (China); Jiangsu Provincial Key Laboratory of Materials Cycling and Pollution Control, Nanjing Normal University, Nanjing 210023 (China); Jiangsu Center for Collaborative Innovation in Geographical Information Resource Development and Application, Nanjing Normal University, Nanjing 210023 (China)

2015-03-30

Graphical abstract: - Highlights: • Poorly crystalline HAP was firstly used for FA removal from aqueous solution. • The maximum adsorption capacity was determined to be 90.20 mg/g at 318 K. • Adsorption kinetics, isotherms and thermodynamic have been studied in detail. • Adsorption mechanism involved surface complexation, electrostatic interaction and hydrogen bonding. - Abstract: In this study, poorly crystalline hydroxyapatite (HAP) was developed as an efficient adsorbent for the removal of fulvic acid (FA) from aqueous solution. Surface functionality, crystallinity, and morphology of the synthetic adsorbent were studied by Fourier-transformation infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effects of various parameters such as crystallinity of adsorbent, contact time, adsorbent dosage, pH, initial adsorbate concentration, temperature, ionic strength and the presence of alkaline earth metal ions on FA adsorption were investigated. Results indicated that the nanosized HAP calcined at lower temperature was poorly crystalline (X{sub c} = 0.23) and had better adsorption capacity for FA than those (X{sub c} = 0.52, 0.86) calcined at higher temperature. FA removal was increased with increases of adsorbent dosage, temperature, ionic strength and the presence of alkali earth metal ions, but decreased as the pH increased. Kinetic studies showed that pseudo-second-order kinetic model better described the adsorption process. Equilibrium data were best described by Sips models, and the estimated maximum adsorption capacity of poorly crystalline HAP was 90.20 mg/g at 318 K, displaying higher efficiency for FA removal than previously reported adsorbents. FT-IR results revealed that FA adsorption over the adsorbent could be attributed to the surface complexation between the oxygen atom of functional groups of FA and calcium ions of HAP. Regeneration studies indicated that HAP could be recyclable for a long

Enhanced oral bioavailability of fenofibrate using polymeric nanoparticulated systems: physicochemical characterization and in vivo investigation

Directory of Open Access Journals (Sweden)

Yousaf AM

2015-03-01

other formulations, it existed in the crystalline state with a reduced intensity. The aqueous solubility and dissolution rates of the nanoparticles (after 30 minutes were not significantly different from one another. Among the nanoparticulated systems tested in this study, the initial dissolution rates (up to 10 minutes were higher with the PVP nanospheres and HP-β-CD nanocorpuscles; however, neither of them resulted in the highest oral bioavailability. Irrespective of relatively retarded dissolution rate, gelatin nanocapsules showed the highest apparent aqueous solubility and furnished the most improved oral bioavailability of the drug (~5.5-fold, owing to better wetting and diminution in crystallinity.Conclusion: Fenofibrate-loaded gelatin nanocapsules prepared using the solvent-evaporation method through the spray-drying technique could be a potential oral pharmaceutical product for administering the poorly water-soluble fenofibrate with an enhanced bioavailability.Keywords: gelatin nanocapsules, hydrophilic polymeric matrix, crystallinity, ameliorated oral bioavailability

Synthesis of mesoporous hydroxyapatite using a modified hard-templating route

International Nuclear Information System (INIS)

Xia Zhiguo; Liao Libing; Zhao Senlin

2009-01-01

Mesoporous polycrystals of hydroxyapatite-calcium are synthesized via a modified hard-templating route. The structure properties of hydroxyapatite-calcium are characterized by means of X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and N 2 adsorption-desorption isotherms. Wide-angle X-ray diffraction and Fourier transform infrared spectroscopy measurements reveal that the crystalline grains consist of highly crystalline pure hydroxyapatite phases. Transmission electron microscopy results show that rod-like hydroxyapatite-calcium grains with an average diameter of about 100 nm long and about 20 nm wide are uniformly distributed, which are also observed with an average pore size of 2-3 nm. Based on N 2 adsorption-desorption isotherms investigation, the pore size, surface area and pore volume of mesoporous hydroxyapatite-calcium are 2.73 nm, 42.43 m 2 g -1 and 0.12 cm 3 g -1 , respectively.

Suspension thermal spraying of hydroxyapatite: Microstructure and in vitro behaviour

Energy Technology Data Exchange (ETDEWEB)

Bolelli, Giovanni, E-mail: giovanni.bolelli@unimore.it [Department of Engineering “Enzo Ferrari”, Università di Modena e Reggio Emilia, Via Vignolese 905, 41125 Modena, MO (Italy); Bellucci, Devis; Cannillo, Valeria; Lusvarghi, Luca; Sola, Antonella [Department of Engineering “Enzo Ferrari”, Università di Modena e Reggio Emilia, Via Vignolese 905, 41125 Modena, MO (Italy); Stiegler, Nico; Müller, Philipp; Killinger, Andreas; Gadow, Rainer [Institute for Manufacturing Technologies of Ceramic Components and Composites (IMTCCC), Universität Stuttgart, Allmandring 7b, 70569 Stuttgart (Germany); Altomare, Lina; De Nardo, Luigi [Dipartimento di Chimica, Materiali e Ingegneria Chimica “G. Natta”, Politecnico di Milano, Via Mancinelli 7, I-20131 Milano (Italy)

2014-01-01

In cementless fixation of metallic prostheses, bony ingrowth onto the implant surface is often promoted by osteoconductive plasma-sprayed hydroxyapatite coatings. The present work explores the use of the innovative High Velocity Suspension Flame Spraying (HVSFS) process to coat Ti substrates with thin homogeneous hydroxyapatite coatings. The HVSFS hydroxyapatite coatings studied were dense, 27–37 μm thick, with some transverse microcracks. Lamellae were sintered together and nearly unidentifiable, unlike conventional plasma-sprayed hydroxyapatite. Crystallinities of 10%–70% were obtained, depending on the deposition parameters and the use of a TiO{sub 2} bond coat. The average hardness of layers with low (< 24%) and high (70%) crystallinity was ≈ 3.5 GPa and ≈ 4.5 GPa respectively. The distributions of hardness values, all characterised by Weibull modulus in the 5–7 range, were narrower than that of conventional plasma-sprayed hydroxyapatite, with a Weibull modulus of ≈ 3.3. During soaking in simulated body fluid, glassy coatings were progressively resorbed and replaced by a new, precipitated hydroxyapatite layer, whereas coatings with 70% crystallinity were stable up to 14 days of immersion. The interpretation of the precipitation behaviour was also assisted by surface charge assessments, performed through Z-potential measurements. During in vitro tests, HA coatings showed no cytotoxicity towards the SAOS-2 osteoblast cell line, and surface cell proliferation was comparable with proliferation on reference polystyrene culture plates. - Highlights: • Thin, dense HA layers were originated by HVSFS deposition of molten agglomerates of ≈ 1 μm. • Tensile adhesion strength of HVSFS HA onto Ti well above the threshold of ISO 13779-2 • Crystallinity (10–70%) is determined by system temperature during deposition. • Crystallinity controls the reactivity during immersion in simulated body fluid. • SAOS-2 osteoblast-like cells adhered well and

Distinct crystallinity and orientations of hydroxyapatite thin films deposited on C- and A-plane sapphire substrates

Science.gov (United States)

Akazawa, Housei; Ueno, Yuko

2014-10-01

We report how the crystallinity and orientation of hydroxyapatite (HAp) films deposited on sapphire substrates depend on the crystallographic planes. Both solid-phase crystallization of amorphous HAp films and crystallization during sputter deposition at elevated temperatures were examined. The low-temperature epitaxial phase on C-plane sapphire substrates has c-axis orientated HAp crystals regardless of the crystallization route, whereas the preferred orientation switches to the (310) direction at higher temperatures. Only the symmetric stretching mode (ν1) of PO43- units appears in the Raman scattering spectra, confirming well-ordered crystalline domains. In contrast, HAp crystals grown on A-plane sapphire substrates are always oriented toward random orientations. Exhibiting all vibrational modes (ν1, ν3, and ν4) of PO43- units in the Raman scattering spectra reflects random orientation, violating the Raman selection rule. If we assume that Raman intensities of PO43- units represent the crystallinity of HAp films, crystallization terminating the surface with the C-plane is hindered by the presence of excess H2O and OH species in the film, whereas crystallization at random orientations on the A-plane sapphire is rather promoted by these species. Such contrasting behaviors between C-plane and A-plane substrates will reflect surface-plane dependent creation of crystalline seeds and eventually determine the orientation of resulting HAp films.

Crystalline hydroxyapatite coatings synthesized under hydrothermal conditions on modified titanium substrates.

Science.gov (United States)

Suchanek, Katarzyna; Bartkowiak, Amanda; Gdowik, Agnieszka; Perzanowski, Marcin; Kąc, Sławomir; Szaraniec, Barbara; Suchanek, Mateusz; Marszałek, Marta

2015-06-01

Hydroxyapatite coatings were successfully produced on modified titanium substrates via hydrothermal synthesis in a Ca(EDTA)(2-) and (NH4)2HPO4 solution. The morphology of modified titanium substrates as well as hydroxyapatite coatings was studied using scanning electron microcopy and phase identification by X-ray diffraction, and Raman and FTIR spectroscopy. The results show that the nucleation and growth of hydroxyapatite needle-like crystals with hexagonal symmetry occurred only on titanium substrates both chemically and thermally treated. No hydroxyapatite phase was detected on only acid etched Ti metal. This finding demonstrates that only a particular titanium surface treatment can effectively induce the apatite nucleation under hydrothermal conditions. Copyright © 2015 Elsevier B.V. All rights reserved.

Finite Element Simulation of Diametral Strength Test of Hydroxyapatite

International Nuclear Information System (INIS)

Ozturk, Fahrettin; Toros, Serkan; Evis, Zafer

2011-01-01

In this study, the diametral strength test of sintered hydroxyapatite was simulated by the finite element software, ABAQUS/Standard. Stress distributions on diametral test sample were determined. The effect of sintering temperature on stress distribution of hydroxyapatite was studied. It was concluded that high sintering temperatures did not reduce the stress on hydroxyapatite. It had a negative effect on stress distribution of hydroxyapatite after 1300 deg. C. In addition to the porosity, other factors (sintering temperature, presence of phases and the degree of crystallinity) affect the diametral strength of the hydroxyapatite.

Suspension thermal spraying of hydroxyapatite: microstructure and in vitro behaviour.

Science.gov (United States)

Bolelli, Giovanni; Bellucci, Devis; Cannillo, Valeria; Lusvarghi, Luca; Sola, Antonella; Stiegler, Nico; Müller, Philipp; Killinger, Andreas; Gadow, Rainer; Altomare, Lina; De Nardo, Luigi

2014-01-01

In cementless fixation of metallic prostheses, bony ingrowth onto the implant surface is often promoted by osteoconductive plasma-sprayed hydroxyapatite coatings. The present work explores the use of the innovative High Velocity Suspension Flame Spraying (HVSFS) process to coat Ti substrates with thin homogeneous hydroxyapatite coatings. The HVSFS hydroxyapatite coatings studied were dense, 27-37μm thick, with some transverse microcracks. Lamellae were sintered together and nearly unidentifiable, unlike conventional plasma-sprayed hydroxyapatite. Crystallinities of 10%-70% were obtained, depending on the deposition parameters and the use of a TiO2 bond coat. The average hardness of layers with low (hydroxyapatite, with a Weibull modulus of ≈3.3. During soaking in simulated body fluid, glassy coatings were progressively resorbed and replaced by a new, precipitated hydroxyapatite layer, whereas coatings with 70% crystallinity were stable up to 14days of immersion. The interpretation of the precipitation behaviour was also assisted by surface charge assessments, performed through Z-potential measurements. During in vitro tests, HA coatings showed no cytotoxicity towards the SAOS-2 osteoblast cell line, and surface cell proliferation was comparable with proliferation on reference polystyrene culture plates. © 2013.

Gel nano-particulates against radioactivity; Des nanoparticules en gel contre la radioactivite

Energy Technology Data Exchange (ETDEWEB)

Deroin, Ph

2004-11-01

The Argonne research center (USA) has developed a 'super-gel' compound, a polymer close to those used in baby's diapers, which can reach a 90% efficiency in the radioactive decontamination of porous materials, like bricks or concrete. The contaminated materials are sprayed with a mixture of polymer gel and wetting agent with nano-particulates in suspension. Under the action of the wetting agent, radioactivity migrates from the pores to the gel and is trapped by the nano-particulates. The drying and recycling of the gel allows to reduce the volume of radioactive wastes. Short paper. (J.S.)

Deposition of Crystalline Hydroxyapatite Nanoparticles on Y-TZP Ceramic: A Potential Solution to Enhance Bonding Characteristics of Y-TZP Ceramics

Directory of Open Access Journals (Sweden)

Abbas Azari

2017-08-01

Full Text Available Objectives: Many advantages have been attributed to dental zirconia ceramics in terms of mechanical and physical properties; however, the bonding ability of this material to dental structure and/or veneering ceramics has always been a matter of concern. On the other hand, hydroxyapatite (HA shows excellent biocompatibility and good bonding ability to tooth structure, with mechanically unstable and brittle characteristics, that make it clinically unacceptable for use in high stress bearing areas. The main purpose of this study was to introduce two simple yet practical methods to deposit the crystalline HA nanoparticles on zirconia ceramics. Materials and Methods: zirconia blocks were treated with HA via two different deposition methods namely thermal coating and air abrasion. Specimens were analyzed by scanning electron microscopy, energy dispersive spectroscopy (EDS and X-ray diffraction (XRD.Results: In both groups, the deposition techniques used were successfully accomplished, while the substrate showed no structural change. However, thermal coating group showed a uniform deposition of crystalline HA but in air abrasion method, there were dispersed thin islands of HA.Conclusions: Thermal coating method has the potential to significantly alter the surface characteristics of zirconia. The simple yet practical nature of the proposed method may be able to shift the bonding paradigm of dental zirconia ceramics. This latter subject needs to be addressed in future investigations.Keywords: Zirconium Oxide; Hydroxyapatites; Dental Bonding; Microscopy, Electron, Scanning; X-Ray Diffraction; Spectrometry, X-Ray Emission

The crystallinity of calcium phosphate powders influenced by the conditions of neutralized procedure with citric acid additions

International Nuclear Information System (INIS)

Li Chengfeng

2009-01-01

Calcium phosphate powders with nano-sized crystallinity were synthesized by neutralization using calcium hydroxide and orthophosphoric acid with the assistance of citric acid. The influence of processing parameters, such as free or additive citric acid, synthetic temperature and ripening time, on the crystallinity of hydroxyapatite were investigated. The results of X-ray diffraction and microstructure observations showed that the crystallinity and morphology of nano-sized hydroxyapatite particles were influenced by the presence or absence of citric acid. It was found that the crystallinities and crystallite sizes of hydroxyapatite powders prepared with the additive citric acid increased with increasing synthetic temperature and ripening time. Especially, the crystallinities of (h k 0) planes were raised and more homogeneously grown particles were obtained with increasing synthetic temperature

Continuous microwave flow synthesis of mesoporous hydroxyapatite.

Science.gov (United States)

Akram, Muhammad; Alshemary, Ammar Z; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O; Hussain, Rafaqat

2015-11-01

We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca(2+) ion released in SBF solution. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and characterization of collagen-hydroxyapatite/pectin composite.

Science.gov (United States)

Wenpo, Feng; Gaofeng, Liang; Shuying, Feng; Yuanming, Qi; Keyong, Tang

2015-03-01

Pectin, a kind of plant polysaccharide, was introduced into collagen-hydroxyapatite composite system, and prepared collagen-hydroxyapatite/pectin (Col-HA/pectin) composite in situ. The structure of the composite was investigated by XRD, SEM, and FT-IR. The mechanical properties, water absorption, enzyme degradation, and cytotoxicity of the composite were investigated as well. The results show that the inorganic substance in the composite materials is hydroxyapatite in relatively low crystallinity. A new interface appeared by the interaction among hydroxyapatite and collagen-pectin, and formed smooth fine particles. The mechanical properties, water absorption, enzyme degradation, and cytotoxicity indicate a potential use in bone replacement for the new composite. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis of nanocrystalline fluorinated hydroxyapatite by ...

Indian Academy of Sciences (India)

The biological hydroxyapatite in the human bone and tooth is of nanosize and ... The crystal size and morphology of the nanopowders were examined by X-ray powder diffraction .... tal growth along the c axis of HA crystalline structure. The.

Influence of spark plasma sintering and baghdadite powder on mechanical properties of hydroxyapatite

NARCIS (Netherlands)

Khandan, A.; Karamian, E.; Mehdikhani-Nahrkhalaji, M.; Mirmohammadi, H.; Farzadi, A.; Ozada, N.; Heidarshenas, B.; Zamani, K.

2015-01-01

Since hydroxyapatite-based materials have similar composition and crystallinity as natural calcified tissues, can be used for bone/tissue engineering. In the present study a novel nanocomposite based on bioceramics such as Natural Hydroxyapatite (NHA) and Baghdadite (BAG), was sintered by spark

Transmission electron microscopy analysis of hydroxyapatite nanocrystals from cattle bones

International Nuclear Information System (INIS)

Patel, Sangeeta; Wei, Shanghai; Han, Jie; Gao, Wei

2015-01-01

In this present study, hydroxyapatite which was obtained from cattle bones has been heat treated at temperature 400 °C and 600 °C. The microstructure after the treatment has been studied in detail using Transmission electron microscopy (TEM) and X-ray diffraction techniques. The TEM results indicate that natural bone consists of collagen and hydroxyapatite nano-crystals which are needle shaped. The heat treatment influences the crystallinity and growth of these hydroxyapatite nano-crystals known as ‘crystal maturation’ or ‘crystal ageing’. - Highlights: • Hydroxyapatite is obtained from cattle bones. • Material has been characterised using XRD and TEM. • Crystal growth and orientation has been studied in detail.

Transmission electron microscopy analysis of hydroxyapatite nanocrystals from cattle bones

Energy Technology Data Exchange (ETDEWEB)

Patel, Sangeeta, E-mail: spt658@aucklanduni.ac.nz [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand); Wei, Shanghai [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand); Han, Jie [Department of Civil and Environmental Engineering, University of Illinois at Urbana-Champaign, 205 North Mathews Avenue, Urbana, IL (United States); Gao, Wei [Department of Chemical and Materials Engineering, The University of Auckland, 20 Symonds Street, Auckland 1010 (New Zealand)

2015-11-15

In this present study, hydroxyapatite which was obtained from cattle bones has been heat treated at temperature 400 °C and 600 °C. The microstructure after the treatment has been studied in detail using Transmission electron microscopy (TEM) and X-ray diffraction techniques. The TEM results indicate that natural bone consists of collagen and hydroxyapatite nano-crystals which are needle shaped. The heat treatment influences the crystallinity and growth of these hydroxyapatite nano-crystals known as ‘crystal maturation’ or ‘crystal ageing’. - Highlights: • Hydroxyapatite is obtained from cattle bones. • Material has been characterised using XRD and TEM. • Crystal growth and orientation has been studied in detail.

Gallium-containing hydroxyapatite for potential use in orthopedics

International Nuclear Information System (INIS)

Melnikov, P.; Teixeira, A.R.; Malzac, A.; Coelho, M. de B.

2009-01-01

A novel material that may be recommended for grafts and implants stimulating bone growth has been obtained by introducing gallium ions (up to 11.0 mass%) into crystalline lattice of hydroxyapatite. The doping was carried out using gallium nitrate and sodium gallate solutions. In both cases, lattice parameters of gallium-doped hydroxyapatite are identical to those of pure synthetic hydroxyapatite. Gallium does not replace calcium as a result of heterovalent substitution and consequently produces no distortions in the framework of hydroxyapatite matrix. It remains strongly fixed in the form of solid solution of intercalation. According to scanning electron microscopy images gallium insertion does not cause any morphological alterations in hydroxyapatite structure and the product developed meets physico-chemical criteria for biomaterial to be employed in orthopedic practice and local handling of traumatic injuries. Its future usage opens the opportunity to enhance osteosynthesis and calcium retention in loco.

Control of composition and crystallinity in hydroxyapatite films deposited by electron cyclotron resonance plasma sputtering

Science.gov (United States)

Akazawa, Housei; Ueno, Yuko

2014-01-01

Hydroxyapatite (HAp) films were deposited by electron cyclotron resonance plasma sputtering under a simultaneous flow of H2O vapor gas. Crystallization during sputter-deposition at elevated temperatures and solid-phase crystallization of amorphous films were compared in terms of film properties. When HAp films were deposited with Ar sputtering gas at temperatures above 460 °C, CaO byproducts precipitated with HAp crystallites. Using Xe instead of Ar resolved the compositional problem, yielding a single HAp phase. Preferentially c-axis-oriented HAp films were obtained at substrate temperatures between 460 and 500 °C and H2O pressures higher than 1×10-2 Pa. The absorption signal of the asymmetric stretching mode of the PO43- unit (ν3) in the Fourier-transform infrared absorption (FT-IR) spectra was the narrowest for films as-crystallized during deposition with Xe, but widest for solid-phase crystallized films. While the symmetric stretching mode of PO43- (ν1) is theoretically IR-inactive, this signal emerged in the FT-IR spectra of solid-phase crystallized films, but was absent for as-crystallized films, indicating superior crystallinity for the latter. The Raman scattering signal corresponding to ν1 PO43- sensitively reflected this crystallinity. The surface hardness of as-crystallized films evaluated by a pencil hardness test was higher than that of solid-phase crystallized films.

Synthesis of hydroxyapatite and structural refinement by X-ray diffraction

International Nuclear Information System (INIS)

Araujo, Jorge Correa de

2007-01-01

A sample of hydroxyapatite was synthesized and its crystalline structure was analyzed by X-ray diffraction by means of the Rietveld method. Two functions were used to fit the peak profiles, modified Voigt (TCHZ) and Pearson VII. The occupational factors and lattice parameters obtained by both models show that the sample does not contain relevant cationic substitutions. The interatomic distances from Ca1 to oxygens O1, O2 and O3 were adequate for a pure hydroxyapatite without defect at site Ca1. Besides, the use of multiple lines in planes (300) and (002) associated with the model Pearson VII resulted in good agreement with the TCHZ model with respect to the size-strain effects with an ellipsoidal shape of crystallites. In conclusion, the procedures adopted in the synthesis of hydroxyapatite produced a pure and crystalline material. The experimental results of transmission electron microscopy confirmed the predicted shape of crystals. (author)

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying

Science.gov (United States)

Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

2015-12-01

Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed.

The precursors effects on biomimetic hydroxyapatite ceramic powders.

Science.gov (United States)

Yoruç, Afife Binnaz Hazar; Aydınoğlu, Aysu

2017-06-01

In this study, effects of the starting material on chemical, physical, and biological properties of biomimetic hydroxyapatite ceramic powders (BHA) were investigated. Characterization and chemical analysis of BHA powders were performed by using XRD, FT-IR, and ICP-AES. Microstructural features such as size and morphology of the resulting BHA powders were characterized by using BET, nano particle sizer, pycnometer, and SEM. Additionally, biological properties of the BHA ceramic powders were also investigated by using water-soluble tetrazolium salts test (WST-1). According to the chemical analysis of BHA ceramic powders, chemical structures of ceramics which are prepared under different conditions and by using different starting materials show differences. Ceramic powders which are produced at 80°C are mainly composed of hydroxyapatite, dental hydroxyapatite (contain Na and Mg elements in addition to Ca), and calcium phosphate sulfide. However, these structures are altered at high temperatures such as 900°C depending on the features of starting materials and form various calcium phosphate ceramics and/or their mixtures such as Na-Mg-hydroxyapatite, hydroxyapatite, Mg-Whitlockit, and chloroapatite. In vitro cytotoxicity studies showed that amorphous ceramics produced at 80°C and ceramics containing chloroapatite structure as main or secondary phases were found to be extremely cytotoxic. Furthermore, cell culture studies showed that highly crystalline pure hydroxyapatite structures were extremely cytotoxic due to their high crystallinity values. Consequently, the current study indicates that the selection of starting materials which can be used in the production of calcium phosphate ceramics is very important. It is possible to produce calcium phosphate ceramics which have sufficient biocompatibility at physiological pH values and by using appropriate starting materials. Copyright © 2017 Elsevier B.V. All rights reserved.

Gel nano-particulates against radioactivity

International Nuclear Information System (INIS)

Deroin, Ph.

2004-01-01

The Argonne research center (USA) has developed a 'super-gel' compound, a polymer close to those used in baby's diapers, which can reach a 90% efficiency in the radioactive decontamination of porous materials, like bricks or concrete. The contaminated materials are sprayed with a mixture of polymer gel and wetting agent with nano-particulates in suspension. Under the action of the wetting agent, radioactivity migrates from the pores to the gel and is trapped by the nano-particulates. The drying and recycling of the gel allows to reduce the volume of radioactive wastes. Short paper. (J.S.)

Biological effects of nanoparticulate materials

International Nuclear Information System (INIS)

Soto, K.F.; Carrasco, A.; Powell, T.G.; Murr, L.E.; Garza, K.M.

2006-01-01

A range of morphologically nanoparticulate materials including Ag, NiO, TiO 2 , multiwall carbon nanotubes, and chrysotile asbestos have been characterized by transmission electron microscopy. All but the TiO 2 (anatase and rutile) were observed to exhibit some cytotoxicity at concentrations of 5 μg/ml for a murine macrophage cell line as a respiratory response model. Silver exhibits interesting systemic differences for animal and human toxicity, especially in light of its nanoparticulate materials, and should be avoided even if there is no detectable in vitro cytotoxic response, as a prudent approach to their technological applications

Synthesis and characterization of hydroxyapatite/alumina ceramic ...

Indian Academy of Sciences (India)

39

In the present work, nano crystalline hydroxyapatite/alumina (HAp-Al2O3) composite was .... powder was dried in hot air oven at 80 °C for 24 hours. ... weekly, and the culture medium was changed twice in a week. 4. Results and Discussion.

Adsorption of nickel on synthetic hydroxyapatite from aqueous solutions

International Nuclear Information System (INIS)

Rosskopfova, O.; Galambos, M.; Pivarciova, L.; Rajec, P.; Caplovicova, M.

2013-01-01

The sorption of nickel on synthetic hydroxyapatite was investigated using a batch method and radiotracer technique. The hydroxyapatite samples used in experiments were a commercial hydroxyapatite and hydroxyapatite of high crystallinity with Ca/P ratio of 1.563 and 1.688, respectively, prepared by a wet precipitation process. The sorption of nickel on hydroxyapatite was pH independent ranging from 4.5 to 6.5 as a result of buffering properties of hydroxyapatite. The adsorption of nickel was rapid and the percentage of Ni sorption on both samples of hydroxyapatite was >98 % during the first 15-30 min of the contact time for initial Ni 2+ concentration of 1 x 10 -4 mol dm -3 . The experimental data for sorption of nickel have been interpreted in the term of Langmuir isotherm and the value of maximum sorption capacity of nickel on a commercial hydroxyapatite and hydroxyapatite prepared by wet precipitation process was calculated to be 0.184 and 0.247 mmol g -1 , respectively. The sorption of Ni 2+ ions was performed by ion-exchange with Ca 2+ cations on the crystal surface of hydroxyapatite under experimental conditions. The competition effect of Co 2+ and Fe 2+ towards Ni 2+ sorption was stronger than that of Ca 2+ ions. NH 4 + ions have no apparent effect on nickel sorption. (author)

Study of sorption processes of copper on synthetic hydroxyapatite

International Nuclear Information System (INIS)

Rosskopfova, O.; Galambos, M.; Ometakova, J.; Rajec, P.; Caplovicova, M.

2012-01-01

The sorption of copper on synthetic hydroxyapatite was investigated using a batch method and radiotracer technique. The hydroxyapatite sample prepared by a wet precipitation process was of high crystallinity with Ca/P ratio of 1.688. The sorption of copper on hydroxyapatite was pH independent ranging from 4 to 6 as a result of buffering properties of hydroxyapatite. The adsorption of copper was rapid and the percentage of Cu sorption was >98% during the first 15-30 min of the contact time. The experimental data for sorption of copper have been interpreted in the term of Langmuir isotherm. The sorption of Cu 2+ ions was performed by ion-exchange with Ca 2+ cations on the crystal surface of hydroxyapatite under experimental conditions. The competition effect of Zn 2+ , Fe 2+ and Pb 2+ towards Cu 2+ sorption was stronger than that of Co 2+ , Ni 2+ and Ca 2+ ions. The ability of the bivalent cations to depress the sorption of copper on hydroxyapatite was in the following order Pb 2+ > Fe 2+ > Zn 2+ > Co 2+ ∼ Ni 2+ . (author)

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying

OpenAIRE

Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

2015-01-01

Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The t...

Surface modification of calcium–copper hydroxyapatites using polyaspartic acid

International Nuclear Information System (INIS)

Othmani, Masseoud; Aissa, Abdallah; Bachoua, Hassen; Debbabi, Mongi

2013-01-01

Highlights: ► The reaction of polyaspartic acid with calcium hydroxyapatite and mixed calcium–copper hydroxyapatite is tested. ► Chemical analysis shows that the presence of copper in the apatitic structure increases the reactivity of the apatite surface. ► X-ray powder analysis shows the conservation of unique crystalline phase of hydroxyapatite after copper incorporation and/or PASP acid reacting. ► IR spectra show the formation of the formation of organometallic bond M-O-C (M=Ca or Cu) on the apatitic surface. ► Transmission electron microscopy (TEM) micrographs and atomic force microscopy (AFM) indicated that the texture surface was changed by the grafting. - Abstract: Mixed calcium–copper hydroxyapatite (Ca–CuHAp), with general formula Ca (10−x) Cu x (PO 4 ) 6 (OH) 2 , where 0 ≤ x ≤ 0.75 was prepared in aqueous medium in the presence of different concentrations of poly-L-aspartic acid (PASP). XRD, IR, TG-DTA, TEM-EDX, AFM and chemical analyses were used to characterize the structure, morphology and composition of the products. All techniques show the formation of new hybrid compounds Ca–CuHAp–PASP. The presence of the grafting moiety on the apatitic material is more significant with increasing of copper amount and/or organic concentration in the starting solution. These increases lead to the affectation of apatite crystallinity. The IR spectroscopy shows the conservation of (P-OH) band of (HPO 4 ) 2− groups, suggesting that PASP acid was interacted only with metallic cations of hydroxyapatite.

Synthesis of fluorapatite–hydroxyapatite nanoparticles and toxicity investigations

Directory of Open Access Journals (Sweden)

N Montazeri

2011-01-01

Full Text Available N Montazeri, R Jahandideh, Esmaeil BiazarDepartment of Chemistry, Islamic Azad University-Tonekabon Branch, Mazandaran, IranAbstract: In this study, calcium phosphate nanoparticles with two phases, fluorapatite (FA; Ca10(PO46F2 and hydroxyapatite (HA; Ca10(PO46(OH2, were prepared using the sol-gel method. Ethyl phosphate, hydrated calcium nitrate, and ammonium fluoride were used, respectively, as P, Ca, and F precursors with a Ca:P ratio of 1:72. Powders obtained from the sol-gel process were studied after they were dried at 80°C and heat treated at 550°C. The degree of crystallinity, particle and crystallite size, powder morphology, chemical structure, and phase analysis were investigated by scanning electron microscopy (SEM, X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, and Zetasizer experiments. The results of XRD analysis and FTIR showed the presence of hydroxyapatite and fluorapatite phases. The sizes of the crystallites estimated from XRD patterns using the Scherrer equation and the crystallinity of the hydroxyapatite phase were about 20 nm and 70%, respectively. Transmission electron microscope and SEM images and Zetasizer experiments showed an average size of 100 nm. The in vitro behavior of powder was investigated with mouse fibroblast cells. The results of these experiments indicated that the powders were biocompatibile and would not cause toxic reactions. These compounds could be applied for hard-tissue engineering.Keywords: fluorapatite, hydroxyapatite, sol-gel, nanoparticles, biocompatibility

A process for the development of strontium hydroxyapatite

International Nuclear Information System (INIS)

Zahra, N; Fayyaz, M; Iqbal, W; Irfan, M; Alam, S

2014-01-01

A procedure for the preparation of Strontium Hydroxyapatite is adapted to produce high purity and better homogeneity ceramic with good Crystallinity. The strontium substituted bone cement has potential for use in orthopedic surgeries. Ionic Strontium (Sr) in humans shares the same physiological pathway as calcium and can be deposited in the mineral structure of the bone. In the present study, a novel concept of preparing Sr-contained Hydroxyapatite bone cement by using a precipitation method is proposed to get an ideal biomaterial that possesses potential degradability and more excellent pharmacological effect. Chemical analysis, Fourier Transform Infra Red analysis and Thermogravimetric/ Differential Scanning Calorimetric studies were conducted on prepared Strontium Hydroxyapatite sample to characterize the incorporation of 15% Sr 2 + into the crystal lattice of Hydroxyapatite. Strontium was quantitatively incorporated into Hydroxyapatite where its substitution for calcium provoked a linear shift of the infrared absorption bands of the hydroxyl and phosphate groups. Thus, the formation of Sr-HAp was confirmed by Chemical Analysis, FT-IR and TGA/DSC results

A process for the development of strontium hydroxyapatite

Science.gov (United States)

Zahra, N.; Fayyaz, M.; Iqbal, W.; Irfan, M.; Alam, S.

2014-06-01

A procedure for the preparation of Strontium Hydroxyapatite is adapted to produce high purity and better homogeneity ceramic with good Crystallinity. The strontium substituted bone cement has potential for use in orthopedic surgeries. Ionic Strontium (Sr) in humans shares the same physiological pathway as calcium and can be deposited in the mineral structure of the bone. In the present study, a novel concept of preparing Sr-contained Hydroxyapatite bone cement by using a precipitation method is proposed to get an ideal biomaterial that possesses potential degradability and more excellent pharmacological effect. Chemical analysis, Fourier Transform Infra Red analysis and Thermogravimetric/ Differential Scanning Calorimetric studies were conducted on prepared Strontium Hydroxyapatite sample to characterize the incorporation of 15% Sr2+ into the crystal lattice of Hydroxyapatite. Strontium was quantitatively incorporated into Hydroxyapatite where its substitution for calcium provoked a linear shift of the infrared absorption bands of the hydroxyl and phosphate groups. Thus, the formation of Sr-HAp was confirmed by Chemical Analysis, FT-IR and TGA/DSC results.

A process for the development of strontium hydroxyapatite

International Nuclear Information System (INIS)

Zahra, N.; Fayyaz, M.; Iqbal, W.; Irfan, M.; Alam, S.

2013-01-01

A procedure for the preparation of Strontium Hydroxyapatite is adapted to produce high purity and better homogeneity ceramic with good Crystallinity. The strontium substituted bone cement has potential for use in orthopedic surgeries. Ionic Strontium (Sr) in humans shares the same physiological pathway as calcium and can be deposited in the mineral structure of the bone. In the present study, a novel concept of preparing Sr-contained Hydroxyapatite bone cement by using a precipitation method is proposed to get an ideal biomaterial that possesses potential degradability and more excellent pharmacological effect. Chemical analysis, Fourier Transform Infra Red analysis and Thermogravimetric/ Differential Scanning Calorimetric studies were conducted on prepared Strontium Hydroxyapatite sample to characterize the incorporation of 15 percentage Sr2+ into the crystal lattice of Hydroxyapatite. Strontium was quantitatively incorporated into Hydroxyapatite where its substitution for calcium provoked a linear shift of the infrared absorption bands of the hydroxyl and phosphate groups. Thus, the formation of Sr-HAp was confirmed by Chemical Analysis, FT-IR and TGA/DSC results. (author)

Bone integration capability of nanopolymorphic crystalline hydroxyapatite coated on titanium implants

Directory of Open Access Journals (Sweden)

Suzuki T

2012-02-01

Full Text Available Masahiro Yamada*, Takeshi Ueno*, Naoki Tsukimura, Takayuki Ikeda, Kaori Nakagawa, Norio Hori, Takeo Suzuki, Takahiro OgawaLaboratory of Bone and Implant Sciences, The Weintraub Center for Reconstructive Biotechnology, Division of Advanced Prosthodontics, Biomaterials and Hospital Dentistry, UCLA School of Dentistry, Los Angeles, CA, USA *These authors contributed equally to this workAbstract: The mechanism by which hydroxyapatite (HA-coated titanium promotes bone–implant integration is largely unknown. Furthermore, refining the fabrication of nanostructured HA to the level applicable to the mass production process for titanium implants is challenging. This study reports successful creation of nanopolymorphic crystalline HA on microroughened titanium surfaces using a combination of flame spray and low-temperature calcination and tests its biological capability to enhance bone–implant integration. Sandblasted microroughened titanium implants and sandblasted + HA-coated titanium implants were subjected to biomechanical and histomorphometric analyses in a rat model. The HA was 55% crystallized and consisted of nanoscale needle-like architectures developed in various diameters, lengths, and orientations, which resulted in a 70% increase in surface area compared to noncoated microroughened surfaces. The HA was free from impurity contaminants, with a calcium/phosphorus ratio of 1.66 being equivalent to that of stoichiometric HA. As compared to microroughened implants, HA-coated implants increased the strength of bone–implant integration consistently at both early and late stages of healing. HA-coated implants showed an increased percentage of bone–implant contact and bone volume within 50 µm proximity of the implant surface, as well as a remarkably reduced percentage of soft tissue intervention between bone and the implant surface. In contrast, bone volume outside the 50 µm border was lower around HA-coated implants. Thus, this study

Surface modification of calcium-copper hydroxyapatites using polyaspartic acid

Energy Technology Data Exchange (ETDEWEB)

Othmani, Masseoud; Aissa, Abdallah; Bachoua, Hassen [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia); Debbabi, Mongi, E-mail: m.debbabi@yahoo.fr [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia)

2013-01-01

Highlights: Black-Right-Pointing-Pointer The reaction of polyaspartic acid with calcium hydroxyapatite and mixed calcium-copper hydroxyapatite is tested. Black-Right-Pointing-Pointer Chemical analysis shows that the presence of copper in the apatitic structure increases the reactivity of the apatite surface. Black-Right-Pointing-Pointer X-ray powder analysis shows the conservation of unique crystalline phase of hydroxyapatite after copper incorporation and/or PASP acid reacting. Black-Right-Pointing-Pointer IR spectra show the formation of the formation of organometallic bond M-O-C (M=Ca or Cu) on the apatitic surface. Black-Right-Pointing-Pointer Transmission electron microscopy (TEM) micrographs and atomic force microscopy (AFM) indicated that the texture surface was changed by the grafting. - Abstract: Mixed calcium-copper hydroxyapatite (Ca-CuHAp), with general formula Ca{sub (10-x)}Cu{sub x}(PO{sub 4}){sub 6}(OH){sub 2}, where 0 {<=} x {<=} 0.75 was prepared in aqueous medium in the presence of different concentrations of poly-L-aspartic acid (PASP). XRD, IR, TG-DTA, TEM-EDX, AFM and chemical analyses were used to characterize the structure, morphology and composition of the products. All techniques show the formation of new hybrid compounds Ca-CuHAp-PASP. The presence of the grafting moiety on the apatitic material is more significant with increasing of copper amount and/or organic concentration in the starting solution. These increases lead to the affectation of apatite crystallinity. The IR spectroscopy shows the conservation of (P-OH) band of (HPO{sub 4}){sup 2-} groups, suggesting that PASP acid was interacted only with metallic cations of hydroxyapatite.

Lecithin-based wet chemical precipitation of hydroxyapatite nanoparticles.

Science.gov (United States)

Michał, Wojasiński; Ewa, Duszyńska; Tomasz, Ciach

Hydroxyapatite Ca 10 (PO 4 ) 6 (OH) 2 nanoparticles have been successfully synthesized by the wet chemical precipitation method at 60 °C in the presence of biocompatible natural surfactant-lecithin. The composition and morphology of nanoparticles of hydroxyapatite synthesized with lecithin (nHAp-PC) was studied by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). Size distribution for nanoparticles was measured by nanoparticle tracking analysis in NanoSight system. We discuss in details influence of lecithin concentration in reaction system on nHAp-PC morphology, as well as on size distributions and suspendability of nanoparticles. Product exhibits crystalline structure and chemical composition of hydroxyapatite, with visible traces of lecithin. Difference in surfactant amounts results in changes in particles morphology and their average size.

Carbonate Hydroxyapatite and Silicon-Substituted Carbonate Hydroxyapatite: Synthesis, Mechanical Properties, and Solubility Evaluations

Directory of Open Access Journals (Sweden)

L. T. Bang

2014-01-01

Full Text Available The present study investigates the chemical composition, solubility, and physical and mechanical properties of carbonate hydroxyapatite (CO3Ap and silicon-substituted carbonate hydroxyapatite (Si-CO3Ap which have been prepared by a simple precipitation method. X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR, X-ray fluorescence (XRF spectroscopy, and inductively coupled plasma (ICP techniques were used to characterize the formation of CO3Ap and Si-CO3Ap. The results revealed that the silicate (SiO44- and carbonate (CO32- ions competed to occupy the phosphate (PO43- site and also entered simultaneously into the hydroxyapatite structure. The Si-substituted CO3Ap reduced the powder crystallinity and promoted ion release which resulted in a better solubility compared to that of Si-free CO3Ap. The mean particle size of Si-CO3Ap was much finer than that of CO3Ap. At 750°C heat-treatment temperature, the diametral tensile strengths (DTS of Si-CO3Ap and CO3Ap were about 10.8±0.3 and 11.8±0.4 MPa, respectively.

Hydroxyapatite nanocrystals: Simple preparation, characterization and formation mechanism

International Nuclear Information System (INIS)

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-01-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ( 1 H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. - Highlights: • HAP nanobundles and nanoparticles have been prepared by a precipitation method. • Morphologies of HAP nanocrystals were controlled by different coordination ligands. • The formation mechanism of hydroxyapatite nanocrystals was also considered

Hydroxyapatite nanocrystals: Simple preparation, characterization and formation mechanism

Energy Technology Data Exchange (ETDEWEB)

Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Fathi, Mohammadhossein [Biomaterials Research Group, Department of Materials Engineering, Isfahan University of Technology, Isfahan 8415683111, Islamic Republic of Iran (Iran, Islamic Republic of); Dental Materials Research Center, Isfahan University of Medical Sciences, Isfahan, Islamic Republic of Iran (Iran, Islamic Republic of); Fereshteh, Zeinab [Biomaterials Research Group, Department of Materials Engineering, Isfahan University of Technology, Isfahan 8415683111, Islamic Republic of Iran (Iran, Islamic Republic of)

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ({sup 1}H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. - Highlights: • HAP nanobundles and nanoparticles have been prepared by a precipitation method. • Morphologies of HAP nanocrystals were controlled by different coordination ligands. • The formation mechanism of hydroxyapatite nanocrystals was also considered.

A comparative study of the metastable equilibrium solubility behavior of high-crystallinity and low-crystallinity carbonated apatites using pH and solution strontium as independent variables.

Science.gov (United States)

Heslop, D D; Bi, Y; Baig, A A; Otsuka, M; Higuchi, W I

2005-09-01

Using solution strontium and pH as independent variables, the metastable equilibrium solubility (MES) behavior of two carbonated apatite (CAP) samples has been examined, a high-crystallinity CAP (properties expected to be similar to dental enamel) and a low-crystallinity CAP (properties expected to be similar to bone mineral). CAP samples were prepared by precipitation/digestion: (CAP A: high-crystallinity, 1.3 wt% CO3, synthesized at 85 degrees C; CAP B: low-crystallinity, 6.4 wt% CO3, synthesized at 50 degrees C). Baseline MES distributions were determined in a series of 0.1 M acetate buffers containing only calcium and phosphate (no strontium) over a broad range of solution conditions. To assess the influence of strontium, MES profiles were determined in a similar fashion with 20, 40, 60, and 80% of the solution calcium being replaced on an equal molar basis by solution strontium. To determine the correct function governing CAP dissolution, ion activity products (IAPs) were calculated from the compositions of buffer solutions based on the hydroxyapatite template (Ca(10-n)Sr(n)(PO4)6(OH)2 (n = 0-10)) and the calcium/hydroxide deficient hydroxyapatite template (Ca(9-n)Sr(n)(HPO4)(PO4)5OH (n = 0-9)). (a) for CAP A, at high solution strontium/calcium ratios, the MES profiles were essentially superimposable when the solution IAPs were calculated using the stoichiometry of Ca6Sr4(PO4)6(OH)2 and for CAP B by a stoichiometry of Ca7Sr2(HPO4)(PO4)5OH; (b) for CAP A, at low strontium/calcium ratios, the stoichiometry yielding MES data superpositioning was found to be that of hydroxyapatite and for CAP B, that of calcium/hydroxide deficient hydroxyapatite. When other stoichiometries were assumed, good superpositioning of the data was not possible.

An ESR study of defects in irradiated hydroxyapatite

International Nuclear Information System (INIS)

Murata, T.; Shiraishi, K.; Ebina, Y.; Miki, T.

1996-01-01

Radiation-induced defects in synthetic hydroxyapatite (HAp) of six different origins have been investigated by electron spin resonance (ESR), X-ray diffraction (XRD), Raman scattering and IR measurements. The orthorhombic CO 2 - radicals were detected in almost all of the samples examined, but the isotropic CO 2 - was produced only in water-containing HAp with low crystallinity. The doublet signal due to H 0 was clearly detected in HAp with extreme calcium deficiency as compared to the stoichiometry. The results of ESR and FTIR suggest that water molecules in low crystalline HAp are not on the surface but embedded in the HAp crystalline lattice. (author)

Synthesis and characterization of magnetite/hydroxyapatite tubes ...

Indian Academy of Sciences (India)

The first step is the formation of magnetite (Fe 3 O 4 ) tubes on natural template followed by hydroxyapatite (HAp) bioceramic coated on the Fe 3 O 4 tubes. HAp improves the biocompatibility and stability of the prepared tubes. Sintering at 900 ∘ C improves the crystalline stability of nanotubes and removes the natural ...

Nano-crystalline thin and nano-particulate thick TiO2 layer: Cost effective sequential deposition and study on dye sensitized solar cell characteristics

International Nuclear Information System (INIS)

Das, P.; Sengupta, D.; Kasinadhuni, U.; Mondal, B.; Mukherjee, K.

2015-01-01

Highlights: • Thin TiO 2 layer is deposited on conducting substrate using sol–gel based dip coating. • TiO 2 nano-particles are synthesized using hydrothermal route. • Thick TiO 2 particulate layer is deposited on prepared thin layer. • Dye sensitized solar cells are made using thin and thick layer based photo-anode. • Introduction of thin layer in particulate photo-anode improves the cell efficiency. - Abstract: A compact thin TiO 2 passivation layer is introduced between the mesoporous TiO 2 nano-particulate layer and the conducting glass substrate to prepare photo-anode for dye-sensitized solar cell (DSSC). In order to understand the effect of passivation layer, other two DSSCs are also developed separately using TiO 2 nano-particulate and compact thin film based photo-anodes. Nano-particles are prepared using hydrothermal synthesis route and the compact passivation layer is prepared by simply dip coating the precursor sol prepared through wet chemical route. The TiO 2 compact layer and the nano-particles are characterised in terms of their micro-structural features and phase formation behavior. It is found that introduction of a compact TiO 2 layer in between the mesoporous TiO 2 nano-particulate layer and the conducting substrate improves the solar to electric conversion efficiency of the fabricated cell. The dense thin passivation layer is supposed to enhance the photo-excited electron transfer and prevent the recombination of photo-excited electrons

In-situ observation of the transformation of amorphous calcium phosphate to crystalline hydroxyapatite

Science.gov (United States)

Stammeier, Jessica; Hippler, Dorothee; Mavromatis, Vasileios; Sacher, Stephan; Dietzel, Martin

2016-04-01

Amorphous calcium phosphate (Ca3(PO4)2*nH2O; ACP) is often a precursor phase of the mineral (hydroxy-) apatite (Ca5(PO4)3(OH)) that can be formed in natural settings during both authigenic and biogenic mineral formation. Particularly, in the biomineralization process of fish tissue, ACP has shown to be an important transient phase. In solution ACP rapidly transforms into the crystalline phase. The transformation rate highly depends on the physico-chemical conditions of the solution: Ca & P availability, pH and temperature. In natural settings Ca can be provided by different sources: from (1) seawater, (2) porewater, or (3) diagenetically-altered carbonates, whereas local supersaturation of P can be induced by microbial activity. In this study, we performed phosphate precipitation experiments in order to monitor the transformation process of the ACP to crystalline hydroxyapatite (HAP) using in-situ Raman spectroscopy. During the experiments the temperature was kept constant at 20.0 ± 0.01 ° C and pH at 9 ± 0.1. 50 ml of 0.3 CaCl 2H2O was titrated at a rate of 5 ml/min to an equal volume of 0.2 M Na2HPO4. The pH was kept constant by titration of 1 M NaOH. During the experiment samples were taken from the solution and instantly filtered. The obtained solid samples were lyophilized and analyzed with XRD, ATR and SEM. The respective solution samples were analyzed using ion chromatography and ICP OES, coupling the spectroscopic data with detailed solution chemistry data. We observed transformation of ACP to HAP to occur within 14 hours, illustrated in a clear peak shift in Raman spectra from 950 cm-1 to 960 cm-1. The obtained results are discussed in the aspects of distribution of major elements during the formation of phosphates and/or the diagenetic alteration of carbonates to phosphates in geologic settings. Financial support by DFG-FG 736 and NAWI Graz is kindly acknowledged.

Topography, wetting, and corrosion responses of electrodeposited hydroxyapatite and fluoridated hydroxyapatite on magnesium.

Science.gov (United States)

Assadian, Mahtab; Jafari, Hassan; Ghaffari Shahri, Seyed Morteza; Idris, Mohd Hasbullah; Almasi, Davood

2016-08-12

In this study, different types of calcium-phosphate phases were coated on NaOH pre-treated pure magnesium. The coating was applied by electrodeposition method in order to provide higher corrosion resistance and improve biocompatibility for magnesium. Thickness, surface morphology and topography of the coatings were analyzed using optical, scanning electron and atomic-force microscopies, respectively. Composition and chemical bonding, crystalline structures and wettability of the coatings were characterized using energy-dispersive and attenuated total reflectance-Fourier transform infrared spectroscopies, grazing incidence X-ray diffraction and contact angle measurement, respectively. Degradation behavior of the coated specimens was also investigated by potentiodynamic polarization and immersion tests. The experiments proved the presence of a porous coating dominated by dicalcium-phosphate dehydrate on the specimens. It was also verified that the developed hydroxyapatite was crystallized by alkali post-treatment. Addition of supplemental fluoride to the coating electrolyte resulted in stable and highly crystallized structures of fluoridated hydroxyapatite. The coatings were found effective to improve biocompatibility combined with corrosion resistance of the specimens. Noticeably, the fluoride supplemented layer was efficient in lowering corrosion rate and increasing surface roughness of the specimens compared to hydroxyapatite and dicalcium-phosphate dehydrates layers.

Microwave annealing for preparation of crystalline hydroxyapatite thin films

CSIR Research Space (South Africa)

Adams, D

2006-11-01

Full Text Available Hydroxyapatite (HA) is widely preferred as the bio- material coating of choice in both dental and ortho- paedic implants due to its favourable osteo-conductive and bioactive properties [1]. Sol–gel synthesis of HA offers a viable alternative to the high... viable option because it is performed in air. Microwave heating differs fundamentally from conventional heating in that heat energy is generated from within the material instead of originating from D. Adams (&) Department of Physics, University...

Synthesis, structural properties and thermal stability of Mn-doped hydroxyapatite

Science.gov (United States)

Paluszkiewicz, Czesława; Ślósarczyk, Anna; Pijocha, Dawid; Sitarz, Maciej; Bućko, Mirosław; Zima, Aneta; Chróścicka, Anna; Lewandowska-Szumieł, Małgorzata

2010-07-01

Hydroxyapatite (HA) - Ca 10(PO 4) 6(OH) 2 is a basic inorganic model component of hard biological tissues, such as bones and teeth. The significant property of HA is its ability to exchange Ca 2+ ions, which influences crystallinity, physico-chemical and biological properties of modified hydroxyapatite materials. In this work, FTIR, Raman spectroscopy, XRD, SEM and EDS techniques were used to determine thermal stability, chemical and phase composition of Mn containing hydroxyapatite (MnHA). Described methods confirmed thermal decomposition and phase transformation of MnHA to αTCP, βTCP and formation of Mn 3O 4 depending on sintering temperature and manganese content. In vitro biological evaluation of Mn-modified HA ceramics was also performed using human osteoblast cells.

Cobalt doped proangiogenic hydroxyapatite for bone tissue engineering application.

Science.gov (United States)

Kulanthaivel, Senthilguru; Roy, Bibhas; Agarwal, Tarun; Giri, Supratim; Pramanik, Krishna; Pal, Kunal; Ray, Sirsendu S; Maiti, Tapas K; Banerjee, Indranil

2016-01-01

The present study delineates the synthesis and characterization of cobalt doped proangiogenic-osteogenic hydroxyapatite. Hydroxyapatite samples, doped with varying concentrations of bivalent cobalt (Co(2+)) were prepared by the ammoniacal precipitation method and the extent of doping was measured by ICP-OES. The crystalline structure of the doped hydroxyapatite samples was confirmed by XRD and FTIR studies. Analysis pertaining to the effect of doped hydroxyapatite on cell cycle progression and proliferation of MG-63 cells revealed that the doping of cobalt supported the cell viability and proliferation up to a threshold limit. Furthermore, such level of doping also induced differentiation of the bone cells, which was evident from the higher expression of differentiation markers (Runx2 and Osterix) and better nodule formation (SEM study). Western blot analysis in conjugation with ELISA study confirmed that the doped HAp samples significantly increased the expression of HIF-1α and VEGF in MG-63 cells. The analysis described here confirms the proangiogenic-osteogenic properties of the cobalt doped hydroxyapatite and indicates its potential application in bone tissue engineering. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparative cytotoxicity assessments of some manufactured and anthropogenic nanoparticulate materials

Science.gov (United States)

Soto, Karla Fabiola

Due to increasing diversity of newly engineered nanoparticles, it is important to consider the hazards of these materials. Very little is known regarding the potential toxicity of relatively new nanomaterials. However, beginning with several historical accounts of nanomaterials applications---chrysotile asbestos and silver---it was assumed that these examples would provide some awareness and guidelines for future nanomaterial and nanotechnology applications, especially health effects. In this study in vitro assays were performed on a murine alveolar macrophage cell line (RAW 264.7), human alveolar macrophage cell line (THB-1), and human epithelial lung cell line (A549) to assess the comparative cytotoxicity of a wide range of manufactured (Ag, TiO2, Fe2O3, Al2O3, ZrO2, black carbon, two different types of multiwall structures and chrysotile asbestos as the toxicity standard) and anthropogenic nanoparticulates. There are several parameters of nanoparticulates that are considered to trigger an inflammatory response (particularly respiratory) or cause toxicity. These parameters include: particle size, shape, specific surface area, transition metals in particulates, and organic compounds. Therefore, a wide variety of manufactured and anthropogenic nanoparticulates having different morphologies, sizes, specific surface area and chemistries as noted were tested. To determine the nanoparticulates' size and morphology, they were characterized by transmission electron microscopy, where it was observed that the commercial multiwall carbon nanotube aggregate had an identical morphology to chrysotile asbestos and combustion-formed carbon nanotubes, i.e.; those that form from natural gas combustion. Light optical microscopy was used to determine cell morphology upon exposure to nanoparticulates as an indication of cell death. Also, the polycyclic aromatic hydrocarbon (PAH) content of the collected nanoparticulates was analyzed and correlated with cytotoxic responses. For

Synthesis of calcium hydrogen phosphate and hydroxyapatite coating on SS316 substrate through pulsed electrodeposition

Energy Technology Data Exchange (ETDEWEB)

Chakraborty, Rajib, E-mail: rajibju4@gmail.com [Department of Mechanical Engineering, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India); Sengupta, Srijan [Department of Metallurgical and Materials Engineering, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India); Saha, Partha [Department of Mechanical Engineering, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India); Das, Karabi; Das, Siddhartha [Department of Metallurgical and Materials Engineering, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India)

2016-12-01

The orthopaedic implants for human body are generally made of different biomaterials like stainless steels or Ti based alloys. However, it has been found that from surface properties point of view, none of these materials is attractive for fast tissue or cell growth on the surface of implant. This is one of the most important criteria to assure quick bonding between implant and body tissues vis-à-vis minimum recovery time for the patient. Keeping in view of the above facts, this work involves the pulsed electro-deposition coating of biocompatible hydroxyapatite and its group compounds from a diluted bath of calcium and phosphate salt at various current densities over the biomaterial sheet of SS316. SEM study confirms different morphologies of the coatings at different current densities. Characterization techniques like X-ray diffraction, SEM with EDX and FTIR have been used to confirm the phase and percentage quantity of hydroxyapatite compound in the depositions. This coating can serve as a medium for faster tissue growth over the metallic implants. - Highlights: • Composite coatings of CaHPO{sub 4} and hydroxyapatite for biomedical application through pulsed electro-deposition. • Achieved optimum phase composition in view of crystallinity of both the phases. • Overall coating crystallinity of around 70% in view better bio compatibility. • In cyclic voltammetry it is observed that the deposition reaction is completely irreversible. • The deposited coating consists of nano-crystalline hydroxyapatite similar to human bone; which exhibits better bio-compatibility.

Hydroxyapatite-Functionalized Graphene: A New Hybrid Nanomaterial

OpenAIRE

Rodríguez-González, C.; Cid-Luna, H. E.; Salas, P.; Castaño, V. M.

2014-01-01

Graphene oxide sheets (GO) were functionalized with hydroxyapatite nanoparticles (nHAp) through a simple and effective hydrothermal treatment and a novel physicochemical process. Microstructure and crystallinity were investigated by Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction (XRD), ultraviolet-visible (UV-Vis) absorption spectroscopy, and thermogravimetric analysis (TGA). Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) ...

Hydrothermal synthesis of hydroxyapatite nanoparticles decorated with silver nanoparticles for application in biomaterials

International Nuclear Information System (INIS)

Assis, Jordanna Fernandes; Arantes, Tatiane Moraes; Cristovan, F.H.; Tada, Dayane Batista

2016-01-01

Full text: The hydroxyapatite nanoparticles (HA) have research attention because are material that exhibit biocompatibility with bone mineral phase of human body is great interest in the scientific community. Synthetic hydroxyapatite nanoparticles have excellent biocompatibility and bioactivity, due biocompatibility and osteo inducibility [1-3]. The hydroxyapatite nanoparticles were synthesized by hydrothermal processing and were characterized by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). The XRD and Raman spectra showed crystalline hydroxyapatite colloidal nanoparticles were obtained in the hexagonal phase. XRD measure showed silver diffraction peaks cubic phase confirmed the presence of the silver nanoparticles decorated hydroxyapatite surface. TEM images showed HA nanoparticles presented a well defined nanorod shapes and narrow size distributions with dimensions (width and length) around of 5 nm and 50 nm decorated with silver nanoparticles of spherical shape about 20 nm in diameter The results showed that crystalline hydroxyapatite colloidal nanoparticles with rod-like morphology and uniform decorated with silver spherical nanoparticles size were obtained by hydrothermal synthesis. These nanoparticles The cell viability of the HA and HA/Ag was analyzed by reduction of the tetrazolium salt (MTT test). Embryonic mouse fibroblast cells were grown in the presence of nanoparticles for a total period of 96 hours. Analyses were made in 24h, 48h, 72h and 96h. The suspensions at the end of each period were analyzed in spectrophotometer. The 24h experiments were the most conclusive, with the silver presence in the HA, there is an increased in cellular proliferation. The results demonstrated that the HA/Ag nanoparticles have potential use as biomaterials in medical/odontological applications. (author)

Hydrothermal synthesis of hydroxyapatite nanoparticles decorated with silver nanoparticles for application in biomaterials

Energy Technology Data Exchange (ETDEWEB)

Assis, Jordanna Fernandes; Arantes, Tatiane Moraes, E-mail: fernandes.jordanna9@gmail.com [Universidade Federal de Goias (UFG), Goiania (Brazil); Cristovan, F.H.; Tada, Dayane Batista [Universidade Federal de Sao Paulo (UNIFESP), Sao Jose dos Campos, SP (Brazil)

2016-07-01

Full text: The hydroxyapatite nanoparticles (HA) have research attention because are material that exhibit biocompatibility with bone mineral phase of human body is great interest in the scientific community. Synthetic hydroxyapatite nanoparticles have excellent biocompatibility and bioactivity, due biocompatibility and osteo inducibility [1-3]. The hydroxyapatite nanoparticles were synthesized by hydrothermal processing and were characterized by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). The XRD and Raman spectra showed crystalline hydroxyapatite colloidal nanoparticles were obtained in the hexagonal phase. XRD measure showed silver diffraction peaks cubic phase confirmed the presence of the silver nanoparticles decorated hydroxyapatite surface. TEM images showed HA nanoparticles presented a well defined nanorod shapes and narrow size distributions with dimensions (width and length) around of 5 nm and 50 nm decorated with silver nanoparticles of spherical shape about 20 nm in diameter The results showed that crystalline hydroxyapatite colloidal nanoparticles with rod-like morphology and uniform decorated with silver spherical nanoparticles size were obtained by hydrothermal synthesis. These nanoparticles The cell viability of the HA and HA/Ag was analyzed by reduction of the tetrazolium salt (MTT test). Embryonic mouse fibroblast cells were grown in the presence of nanoparticles for a total period of 96 hours. Analyses were made in 24h, 48h, 72h and 96h. The suspensions at the end of each period were analyzed in spectrophotometer. The 24h experiments were the most conclusive, with the silver presence in the HA, there is an increased in cellular proliferation. The results demonstrated that the HA/Ag nanoparticles have potential use as biomaterials in medical/odontological applications. (author)

A novel electrospun silk fibroin/hydroxyapatite hybrid nanofibers

International Nuclear Information System (INIS)

Ming, Jinfa; Zuo, Baoqi

2012-01-01

A novel electrospinning of silk fibroin/hydroxyapatite hybrid nanofibers with different composition ratios was performed with methanoic acid as a spinning solvent. The silk fibroin/hydroxyapatite hybrids containing up to 30% hydroxyapatite nanoparticles could be electrospun into the continuous fibrous structure. The electrospun silk fibroin/hydroxyapatite hybrid nanofibers showed bigger diameter and wider diameter distribution than pure silk fibroin nanofibers, and the average diameter gradually increased from 95 to 582 nm. At the same time, the secondary structure of silk fibroin/hydroxyapatite nanofibers was characterized by X-ray diffraction, Fourier transform infrared analysis, and DSC measurement. Comparing with the pure silk fibroin nanofibers, the crystal structure of silk fibroin was mainly amorphous structure in the hybrid nanofibers. X-ray diffraction results demonstrated the hydroxyapatite crystalline nature remained as evidenced from the diffraction planes (002), (211), (300), and (202) of the hydroxyapatite crystallites, which was also confirmed by Fourier transform infrared analysis. The thermal behavior of hybrid nanofibers exhibited the endothermic peak of moisture evaporation ranging from 86 to 113 °C, and the degradation peak at 286 °C appeared. The SF/HAp nanofibers mats containing 30% HAp nanoparticles showed higher breaking tenacity and extension at break for 1.1688 ± 0.0398 MPa and 6.55 ± 1.95%, respectively. Therefore, the electrospun silk fibroin/hydroxyapatite hybrid nanofibers should be provided potentially useful options for the fabrication of biomaterial scaffolds for bone tissue engineering. -- Highlights: ► The novel SF/HAp nanofibers were directly prepared by electrospinning method. ► The nanofiber diameter had significant related to the content of HAp. ► The crystal structure of silk fibroin was mainly amorphous structure in the hybrid nanofibers. ► The HAp crystals existing in the hybrid nanofibers were characterized

Bioceramics synthesis of hydroxyapatite from red snapper fish scales biowaste using wet chemical precipitation route

Science.gov (United States)

Ulfyana, D.; Anugroho, F.; Sumarlan, S. H.; Wibisono, Y.

2018-03-01

Fish scales biowaste contain high collagens and calcium phosphates, therefore have considerable potential as raw material for value-added biomaterial such as hydroxyapatite (HAp). HAp is the main constituent component of hard tissue such as bone and teeth in the human body and is known as bioceramic materials. In this work, wet chemical precipitation method was used to syntesize HAp from Red Snapper Fish (Lutjanus campechanus) Scales. Two variations of calcination temperatures of 600°C (FHAp1) and 800°C (FHAp2) were conducted for 5 hours. The results showed calcium content from biowaste of red snapper fish scale was 83.62%. FTIR result shows that PO4 3-, OH-, and CO3 2- functional groups presence as indicates the formation of HAp. XRD result showed the degree of crystallinity for FHAp1 and FHAp2 were 75.52% and 79.20%, respectively. The degree of crystallinity is in accordance with ISO 13779-2:2000 standard in which the minimum degree of crystallinity of hydroxyapatite used for biomedical materials is 45%. Finally, Particle Size Analyzer (PSA) results show that the particle size distribution is evenly distributed, with the size of micro-scale hydroxyapatite particles, ranging from 5.76 μm to 132.64 μm.

Nano-crystalline thin and nano-particulate thick TiO{sub 2} layer: Cost effective sequential deposition and study on dye sensitized solar cell characteristics

Energy Technology Data Exchange (ETDEWEB)

Das, P.; Sengupta, D. [Centre for Advanced Materials Processing, CSIR-Central Mechanical Engineering Research Institute, Durgapur, 713209 West Bengal (India); CSIR-Central Mechanical Engineering Research Institute, Academy of Scientific and Innovative Research (AcSIR), Durgapur, 713209 West Bengal (India); Kasinadhuni, U. [Department of Engineering Physics, Bengal College of Engineering and Technology, Durgapur, West Bengal (India); Mondal, B. [Centre for Advanced Materials Processing, CSIR-Central Mechanical Engineering Research Institute, Durgapur, 713209 West Bengal (India); Mukherjee, K., E-mail: kalisadhanm@yahoo.com [Centre for Advanced Materials Processing, CSIR-Central Mechanical Engineering Research Institute, Durgapur, 713209 West Bengal (India)

2015-06-15

Highlights: • Thin TiO{sub 2} layer is deposited on conducting substrate using sol–gel based dip coating. • TiO{sub 2} nano-particles are synthesized using hydrothermal route. • Thick TiO{sub 2} particulate layer is deposited on prepared thin layer. • Dye sensitized solar cells are made using thin and thick layer based photo-anode. • Introduction of thin layer in particulate photo-anode improves the cell efficiency. - Abstract: A compact thin TiO{sub 2} passivation layer is introduced between the mesoporous TiO{sub 2} nano-particulate layer and the conducting glass substrate to prepare photo-anode for dye-sensitized solar cell (DSSC). In order to understand the effect of passivation layer, other two DSSCs are also developed separately using TiO{sub 2} nano-particulate and compact thin film based photo-anodes. Nano-particles are prepared using hydrothermal synthesis route and the compact passivation layer is prepared by simply dip coating the precursor sol prepared through wet chemical route. The TiO{sub 2} compact layer and the nano-particles are characterised in terms of their micro-structural features and phase formation behavior. It is found that introduction of a compact TiO{sub 2} layer in between the mesoporous TiO{sub 2} nano-particulate layer and the conducting substrate improves the solar to electric conversion efficiency of the fabricated cell. The dense thin passivation layer is supposed to enhance the photo-excited electron transfer and prevent the recombination of photo-excited electrons.

Novel synthesis and characterization of an AB-type carbonate-substituted hydroxyapatite.

Science.gov (United States)

Gibson, Iain R; Bonfield, William

2002-03-15

A novel synthesis route has been developed to produce a high-purity mixed AB-type carbonate-substituted hydroxyapatite (CHA) with a carbonate content that is comparable to the type and level observed in bone mineral. This method involves the aqueous precipitation in the presence of carbonate ions in solution of a calcium phosphate apatite with a Ca/P molar ratio greater than the stoichiometric value of 1.67 for hydroxyapatite (HA). The resulting calcium-rich carbonate-apatite is sintered/heat-treated in a carbon dioxide atmosphere to produce a single-phase, crystalline carbonate-substituted hydroxyapatite. In contrast to previous methods for producing B- or AB-type carbonate-substituted hydroxyapatites, no sodium or ammonium ions, which would be present in the reaction mixture from the sodium or ammonium carbonates commonly used as a source of carbonate ions, were present in the final product. The chemical and phase compositions of the carbonate-substituted hydroxyapatite was characterized by X-ray fluorescence and X-ray diffraction, respectively, and the level and nature of the carbonate substitution were studied using C-H-N analysis and Fourier transform infrared spectroscopy, respectively. The carbonate substitution improves the densification of hydroxyapatite and reduces the sintering temperature required to achieve near-full density by approximately 200 degrees C compared to stoichiometric HA. Initial studies have shown that these carbonate-substituted hydroxyapatites have improved mechanical and biologic properties compared to stoichiometric hydroxyapatite. Copyright 2001 John Wiley & Sons, Inc. J Biomed Mater Res 59: 697-708, 2002

Cobalt doped proangiogenic hydroxyapatite for bone tissue engineering application

International Nuclear Information System (INIS)

Kulanthaivel, Senthilguru; Roy, Bibhas; Agarwal, Tarun; Giri, Supratim; Pramanik, Krishna; Pal, Kunal; Ray, Sirsendu S.; Maiti, Tapas K.; Banerjee, Indranil

2016-01-01

ABSTRACT: The present study delineates the synthesis and characterization of cobalt doped proangiogenic–osteogenic hydroxyapatite. Hydroxyapatite samples, doped with varying concentrations of bivalent cobalt (Co"2"+) were prepared by the ammoniacal precipitation method and the extent of doping was measured by ICP–OES. The crystalline structure of the doped hydroxyapatite samples was confirmed by XRD and FTIR studies. Analysis pertaining to the effect of doped hydroxyapatite on cell cycle progression and proliferation of MG-63 cells revealed that the doping of cobalt supported the cell viability and proliferation up to a threshold limit. Furthermore, such level of doping also induced differentiation of the bone cells, which was evident from the higher expression of differentiation markers (Runx2 and Osterix) and better nodule formation (SEM study). Western blot analysis in conjugation with ELISA study confirmed that the doped HAp samples significantly increased the expression of HIF-1α and VEGF in MG-63 cells. The analysis described here confirms the proangiogenic–osteogenic properties of the cobalt doped hydroxyapatite and indicates its potential application in bone tissue engineering. - Highlights: • Cobalt (Co"+"2) doped hydroxyapatite (Co-HAp) can be prepared by the wet chemical method. • The concentration of Co"+"2 influences the physico-chemical properties of HAp. • Co-HAp was found to be biocompatible and osteogenic. • Co-HAp enhanced cellular VEGF secretion through HIF-1α stabilization. • The optimum biological performance of Co-HAp was achieved for 0.33% (w/w) Co"+"2 doping.

Iron inhibits hydroxyapatite crystal growth in vitro.

Science.gov (United States)

Guggenbuhl, Pascal; Filmon, Robert; Mabilleau, Guillaume; Baslé, Michel F; Chappard, Daniel

2008-07-01

Hemochromatosis is a known cause of osteoporosis in which the pathophysiology of bone loss is largely unknown and the role of iron remains questionable. We have investigated the effects of iron on the growth of hydroxyapatite crystals in vitro on carboxymethylated poly(2-hydroxyethyl methacrylate) pellets. This noncellular and enzyme-independent model mimics the calcification of woven bone (composed of calcospherites made of hydroxyapatite crystals). Polymer pellets were incubated with body fluid containing iron at increasing concentrations (20, 40, 60 micromol/L). Hydroxyapatite growth was studied by chemical analysis, scanning electron microscopy, and Raman microscopy. When incubated in body fluid containing iron, significant differences were observed with control pellets. Iron was detected at a concentration of 5.41- to 7.16-fold that of controls. In pellets incubated with iron, there was a approximately 3- to 4-fold decrease of Ca and P and a approximately 1.3- to 1.4-fold increase in the Ca/P ratio. There was no significant difference among the iron groups of pellets, but a trend to a decrease of Ca with the increase of iron concentration was noted. Calcospherite diameters were significantly lower on pellets incubated with iron. Raman microspectroscopy showed a decrease in crystallinity (measured by the full width of the half height of the 960 Deltacm(-1) band) with a significant increase in carbonate substitution (measured by the intensity ratio of 1071 to 960 Deltacm(-1) band). Energy dispersive x-ray analysis identified iron in the calcospherites. In vitro, iron is capable to inhibit bone crystal growth with significant changes in crystallinity and carbonate substitution.

Degradation Studies of Polyolefins Incorporating Transparent Nanoparticulate Zinc Oxide UV Stabilizers

International Nuclear Information System (INIS)

Ammala, A.; Hill, A.J.; Meakin, P.; Pas, S.J.; Turney, T.W.

2002-01-01

Coated and dispersed nanoparticulate zinc oxide is shown to improve ultra violet (UV) stability of polypropylene and high-density polyethylene without changing its characteristic absorption spectrum in the visible region (400-800-nm). The performance of these nanoparticulate UV stabilizers is compared to conventional hindered amine light stabilizers (HALS). QUV accelerated weathering is used to simulate long-term exposure. Positron annihilation lifetime spectroscopy (PALS) is used to provide an indication of physical and chemical changes due to accelerated weathering and is shown to have potential for detecting changes well before other techniques. Visual observation, optical microscopy, carbonyl index, yellowness index and PALS indicate that nanoparticulate zinc oxide gives superior resistance to UV degradation compared to organic HALS at appropriate loading levels

Bone integration capability of nanopolymorphic crystalline hydroxyapatite coated on titanium implants

OpenAIRE

Ogawa, Takahiro; Yamada,Masahiro; Ueno,; Tsukimura,Naoki; Ikeda,; Nakagawa,; Hori,; Suzuki,

2012-01-01

Masahiro Yamada*, Takeshi Ueno*, Naoki Tsukimura, Takayuki Ikeda, Kaori Nakagawa, Norio Hori, Takeo Suzuki, Takahiro OgawaLaboratory of Bone and Implant Sciences, The Weintraub Center for Reconstructive Biotechnology, Division of Advanced Prosthodontics, Biomaterials and Hospital Dentistry, UCLA School of Dentistry, Los Angeles, CA, USA *These authors contributed equally to this workAbstract: The mechanism by which hydroxyapatite (HA)-coated titanium promotes bone–implant integratio...

Nanoparticulate delivery systems for antiviral drugs.

Science.gov (United States)

Lembo, David; Cavalli, Roberta

2010-01-01

Nanomedicine opens new therapeutic avenues for attacking viral diseases and for improving treatment success rates. Nanoparticulate-based systems might change the release kinetics of antivirals, increase their bioavailability, improve their efficacy, restrict adverse drug side effects and reduce treatment costs. Moreover, they could permit the delivery of antiviral drugs to specific target sites and viral reservoirs in the body. These features are particularly relevant in viral diseases where high drug doses are needed, drugs are expensive and the success of a therapy is associated with a patient's adherence to the administration protocol. This review presents the current status in the emerging area of nanoparticulate delivery systems in antiviral therapy, providing their definition and description, and highlighting some peculiar features. The paper closes with a discussion on the future challenges that must be addressed before the potential of nanotechnology can be translated into safe and effective antiviral formulations for clinical use.

Tensile properties and microstructural analysis of spheroidized hydroxyapatite-poly (etheretherketone) biocomposites

International Nuclear Information System (INIS)

Abu Bakar, M.S.; Cheang, P.; Khor, K.A.

2003-01-01

Poly(etheretherketone) or PEEK, is a high performance thermoplastic possessing exceptional mechanical properties, high temperature durability, good chemical and fatigue resistance. These coupled with its ability to withstand sterilization treatment, make it a preferred material for biomedical applications. This study examines the benefit of incorporating hydroxyapatite particulates in poly(etheretherketone) for possible usage as bone analogue materials. Flame spheroidized hydroxyapatite (FSHA) were incorporated into semi-crystalline poly(etheretherketone) polymer through a series of processes comprising melt compounding, granulating and injection molding. Biocomposites with high hydroxyapatite loading of up to 40 vol.% were processed successfully using this technique. Scanning electron microscopy (SEM) revealed fair dispersion and distribution of hydroxyapatite particles within the polymer matrix. The series of composites were characterized in terms of tensile and microhardness properties. Microstructural analysis was also carried out to correlate the structure-property relationship of the composite. The dependency of tensile properties such as modulus, strength and strain to fracture as well as the micro-hardness on the volume percentage of hydroxyapatite were investigated. By varying the amount of hydroxyapatite particles in the composite, a wide range of mechanical properties were obtained. In general, the tensile modulus and microhardness increased, while strength and strain to fracture decreased correspondingly with progressive addition of hydroxyapatite particles. The composite system under investigation also exhibited mechanical properties matching those of human bone. With hydroxyapatite loading beyond 30 vol.%, the modulus were within the bounds of the human cortical bone. Findings from this study suggest that this bioactive composite system have the potential as an alternative implant material for orthopaedic application

Bioavailability of nanoparticulate hematite to Arabidopsis thaliana

International Nuclear Information System (INIS)

Marusenko, Yevgeniy; Shipp, Jessie; Hamilton, George A.; Morgan, Jennifer L.L.; Keebaugh, Michael; Hill, Hansina; Dutta, Arnab; Zhuo, Xiaoding; Upadhyay, Nabin; Hutchings, James; Herckes, Pierre; Anbar, Ariel D.; Shock, Everett; Hartnett, Hilairy E.

2013-01-01

The environmental effects and bioavailability of nanoparticulate iron (Fe) to plants are currently unknown. Here, plant bioavailability of synthesized hematite Fe nanoparticles was evaluated using Arabidopsis thaliana (A. thaliana) as a model. Over 56-days of growing wild-type A. thaliana, the nanoparticle-Fe and no-Fe treatments had lower plant biomass, lower chlorophyll concentrations, and lower internal Fe concentrations than the Fe-treatment. Results for the no-Fe and nanoparticle-Fe treatments were consistently similar throughout the experiment. These results suggest that nanoparticles (mean diameter 40.9 nm, range 22.3–67.0 nm) were not taken up and therefore not bioavailable to A. thaliana. Over 14-days growing wild-type and transgenic (Type I/II proton pump overexpression) A. thaliana, the Type I plant grew more than the wild-type in the nanoparticle-Fe treatment, suggesting Type I plants cope better with Fe limitation; however, the nanoparticle-Fe and no-Fe treatments had similar growth for all plant types. -- Highlights: ► Iron nanoparticles were synthesized and assessed for bioavailability to Arabidopsis. ► Arabidopsis grew better in the presence of EDTA-bound iron than nanoparticulate iron. ► Arabidopsis grew the same in the presence of nanoparticulate iron compared to no iron. -- Synthesized iron nanoparticles were not bioavailable to Arabidopsis thaliana in agar nutrient media

Cobalt doped proangiogenic hydroxyapatite for bone tissue engineering application

Energy Technology Data Exchange (ETDEWEB)

Kulanthaivel, Senthilguru [Department of Biotechnology and Medical Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India); Roy, Bibhas [Department of Biotechnology, Indian Institute of Technology Kharagpur, Kharagpur, West Bengal 721302 (India); Agarwal, Tarun [Department of Biotechnology and Medical Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India); Giri, Supratim [Department of Chemistry, National Institute of Technology, Rourkela, Odisha 769008 (India); Pramanik, Krishna; Pal, Kunal; Ray, Sirsendu S. [Department of Biotechnology and Medical Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India); Maiti, Tapas K. [Department of Biotechnology, Indian Institute of Technology Kharagpur, Kharagpur, West Bengal 721302 (India); Banerjee, Indranil, E-mail: indraniliit@gmail.com [Department of Biotechnology and Medical Engineering, National Institute of Technology, Rourkela, Odisha 769008 (India)

2016-01-01

ABSTRACT: The present study delineates the synthesis and characterization of cobalt doped proangiogenic–osteogenic hydroxyapatite. Hydroxyapatite samples, doped with varying concentrations of bivalent cobalt (Co{sup 2+}) were prepared by the ammoniacal precipitation method and the extent of doping was measured by ICP–OES. The crystalline structure of the doped hydroxyapatite samples was confirmed by XRD and FTIR studies. Analysis pertaining to the effect of doped hydroxyapatite on cell cycle progression and proliferation of MG-63 cells revealed that the doping of cobalt supported the cell viability and proliferation up to a threshold limit. Furthermore, such level of doping also induced differentiation of the bone cells, which was evident from the higher expression of differentiation markers (Runx2 and Osterix) and better nodule formation (SEM study). Western blot analysis in conjugation with ELISA study confirmed that the doped HAp samples significantly increased the expression of HIF-1α and VEGF in MG-63 cells. The analysis described here confirms the proangiogenic–osteogenic properties of the cobalt doped hydroxyapatite and indicates its potential application in bone tissue engineering. - Highlights: • Cobalt (Co{sup +2}) doped hydroxyapatite (Co-HAp) can be prepared by the wet chemical method. • The concentration of Co{sup +2} influences the physico-chemical properties of HAp. • Co-HAp was found to be biocompatible and osteogenic. • Co-HAp enhanced cellular VEGF secretion through HIF-1α stabilization. • The optimum biological performance of Co-HAp was achieved for 0.33% (w/w) Co{sup +2} doping.

Analysis of the thermoluminescent signal in the hydroxyapatite synthesized by the sol-gel method

International Nuclear Information System (INIS)

Mendoza A, D.; Gonzalez, P.R.; Lobato, M.; Rubio, E.; Rodriguez L, V.; Custodio, E.

2004-01-01

The physical properties of the ceramics are related with the chemical bonds and the crystalline structure, because the elements that constitute it can be united by ionic bonds or partially ionic giving a covalent character, this last causes that the outer layer is full of electrons. This property makes that the ceramic ones become interesting materials for thermoluminescent applications, as it demonstrates through the recent works presented on the hydroxyapatite that is a ceramic biomaterials that has shown an interesting thermoluminescent signal when being exposed to gamma radiation. In this sense, this work presents the thermoluminescent signal analysis induced by the UV and gamma radiation in a particular type of hydroxyapatite synthesized by sol gel method in which the temperature synthesis is varied. The final thermoluminescent sensitivity of materials is correlated with the crystalline degree, which is analysed through X-ray diffraction. (Author)

Containment of uranium in the proposed Egyptian geologic repository for radioactive waste using hydroxyapatite

International Nuclear Information System (INIS)

Moore, Robert Charles; Hasan, Ahmed Ali Mohamed; Headley, Thomas Jeffrey; Sanchez, Charles Anthony; Zhao, Hongting; Salas, Fred Manuel; Hasan, Mahmoud A.; Holt, Kathleen Caroline

2003-01-01

Currently, the Egyptian Atomic Energy Authority is designing a shallow-land disposal facility for low-level radioactive waste. To insure containment and prevent migration of radionuclides from the site, the use of a reactive backfill material is being considered. One material under consideration is hydroxyapatite, Ca 10 (PO 4 ) 6 (OH) 2 , which has a high affinity for the sorption of many radionuclides. Hydroxyapatite has many properties that make it an ideal material for use as a backfill including low water solubility (K sp > 10 -40 ), high stability under reducing and oxidizing conditions over a wide temperature range, availability, and low cost. However, there is often considerable variation in the properties of apatites depending on source and method of preparation. In this work, we characterized and compared a synthetic hydroxyapatite with hydroxyapatites prepared from cattle bone calcined at 500 C, 700 C, 900 C and 1100 C. The analysis indicated the synthetic hydroxyapatite was similar in morphology to 500 C prepared cattle hydroxyapatite. With increasing calcination temperature the crystallinity and crystal size of the hydroxyapatites increased and the BET surface area and carbonate concentration decreased. Batch sorption experiments were performed to determine the effectiveness of each material to sorb uranium. Sorption of U was strong regardless of apatite type indicating all apatite materials evaluated. Sixty day desorption experiments indicated desorption of uranium for each hydroxyapatite was negligible.

Containment of uranium in the proposed Egyptian geologic repository for radioactive waste using hydroxyapatite

International Nuclear Information System (INIS)

Moore, Robert Charles; Hasan, Ahmed Ali Mohamed; Headley, Thomas Jeffrey; Sanchez, Charles Anthony; Zhao, Hongting; Salas, Fred Manuel; Hasan, Mahmoud A.; Holt, Kathleen Caroline

2004-01-01

Currently, the Egyptian Atomic Energy Authority is designing a shallow-land disposal facility for low-level radioactive waste. To insure containment and prevent migration of radionuclides from the site, the use of a reactive backfill material is being considered. One material under consideration is hydroxyapatite, Ca 10 (PO 4 ) 6 (OH) 2 , which has a high affinity for the sorption of many radionuclides. Hydroxyapatite has many properties that make it an ideal material for use as a backfill including low water solubility (K sp >10 -40 ), high stability under reducing and oxidizing conditions over a wide temperature range, availability, and low cost. However, there is often considerable variation in the properties of apatites depending on source and method of preparation. In this work, we characterized and compared a synthetic hydroxyapatite with hydroxyapatites prepared from cattle bone calcined at 500 C, 700 C, 900 C and 1100 C. The analysis indicated the synthetic hydroxyapatite was similar in morphology to 500 C prepared cattle hydroxyapatite. With increasing calcination temperature the crystallinity and crystal size of the hydroxyapatites increased and the BET surface area and carbonate concentration decreased. Batch sorption experiments were performed to determine the effectiveness of each material to sorb uranium. Sorption of U was strong regardless of apatite type indicating all apatite materials evaluated. Sixty day desorption experiments indicated desorption of uranium for each hydroxyapatite was negligible

Chemical components, pharmacological properties, and nanoparticulate delivery systems of Brucea javanica

Directory of Open Access Journals (Sweden)

Peng X

2013-01-01

Full Text Available Meiwan Chen,1,‡ Ruie Chen,1,‡ Shengpeng Wang,1 Wen Tan,1 Yangyang Hu,1 Xinsheng Peng,2 Yitao Wang11State Key Laboratory of Quality Research in Chinese Medicine, Institute of Chinese Medical Sciences, University of Macau, Macau, China; 2School of Pharmaceutical Sciences, Guangdong Medical College, Dongguan, China‡These authors contributed equally to this workAbstract: Brucea javanica has demonstrated a variety of antitumoral, antimalarial, and anti-inflammatory properties. As a Chinese herbal medicine, Brucea javanica is mainly used in the treatment of lung and gastrointestinal cancers. Pharmacological research has identified the main antitumor components are tetracyclic triterpene quassinoids. However, most of these active components have poor water solubility and low bioavailability, which greatly limit their clinical application. Nanoparticulate delivery systems are urgently needed to improve the bioavailability of Brucea javanica. This paper mainly focuses on the chemical components in Brucea javanica and its pharmacological properties and nanoparticulate formulations, in an attempt to encourage further research on its active components and nanoparticulate drug delivery systems to expand its clinical applications. It is expected to improve the level of pharmaceutical research and provide a strong scientific foundation for further study on the medicinal properties of this plant.Keywords: Brucea javanica, chemical components, pharmacology, nanoparticulate delivery systems

Dual responsive dysprosium-doped hydroxyapatite particles and toxicity reduction after functionalization with folic and glucuronic acids

Energy Technology Data Exchange (ETDEWEB)

Sánchez Lafarga, Ana Karen; Pacheco Moisés, Fermín P. [Departamento de Química, Universidad de Guadalajara, Marcelino García Barragán 1421, C.P. 44430, Guadalajara, Jalisco (Mexico); Gurinov, Andrey [Research Resources Center for Magnetic Resonance, Saint Petersburg State University, Universitetskij pr. 26, 198504 St. Petersburg (Russian Federation); Ortiz, Genaro Gabriel [Laboratorio Desarrollo-Envejecimiento, Enfermedades Neurodegenerativas, Centro de Investigación Biomédica de Occidente (CIBO), Instituto Mexicano de Seguro Social (IMSS), Guadalajara, Jalisco (Mexico); Carbajal Arízaga, Gregorio Guadalupe, E-mail: gregoriocarbajal@yahoo.com.mx [Departamento de Química, Universidad de Guadalajara, Marcelino García Barragán 1421, C.P. 44430, Guadalajara, Jalisco (Mexico)

2015-03-01

The development of probes for biomedical applications demands materials with low toxicity levels besides fluorescence or magnetic properties to be detected by confocal microscopes or MRI resonators. Several drug delivery systems or other biomedical materials prepared with hydroxyapatite have been proposed, however, toxicity effects might arise when the size of particles is nanometric. In this study, hydroxyapatite functionalized with glucuronic or folic acids presented lower oxidative stress, measured from lipoperoxides and nitric oxide indicators in rats than pure hydroxyapatite. In separated experiments, hydroxyapatite was doped with dysprosium cations by coprecipitation producing a single crystal phase with fluorescent properties easily visualized by confocal microscopy when excited at 488 nm. These particles also presented the ability to modify the proton relaxation time in T1 maps collected by magnetic resonance imaging. These modified hydroxyapatite nanoparticles could be candidates to design bimodal probes with low toxicity. - Highlights: • Hydroxyapatite functionalized with glucuronic acid reduced oxidative stress in rats. • Functionalization with folic acid reduced oxidative stress in rats. • Dysprosium doping does not affect the crystalline structure of hydroxyapatite. • Dysprosium doped particles are visible in fluorescent microscope. • Dysprosium doped particles act as MRI contrast agents.

Dual responsive dysprosium-doped hydroxyapatite particles and toxicity reduction after functionalization with folic and glucuronic acids

International Nuclear Information System (INIS)

Sánchez Lafarga, Ana Karen; Pacheco Moisés, Fermín P.; Gurinov, Andrey; Ortiz, Genaro Gabriel; Carbajal Arízaga, Gregorio Guadalupe

2015-01-01

The development of probes for biomedical applications demands materials with low toxicity levels besides fluorescence or magnetic properties to be detected by confocal microscopes or MRI resonators. Several drug delivery systems or other biomedical materials prepared with hydroxyapatite have been proposed, however, toxicity effects might arise when the size of particles is nanometric. In this study, hydroxyapatite functionalized with glucuronic or folic acids presented lower oxidative stress, measured from lipoperoxides and nitric oxide indicators in rats than pure hydroxyapatite. In separated experiments, hydroxyapatite was doped with dysprosium cations by coprecipitation producing a single crystal phase with fluorescent properties easily visualized by confocal microscopy when excited at 488 nm. These particles also presented the ability to modify the proton relaxation time in T1 maps collected by magnetic resonance imaging. These modified hydroxyapatite nanoparticles could be candidates to design bimodal probes with low toxicity. - Highlights: • Hydroxyapatite functionalized with glucuronic acid reduced oxidative stress in rats. • Functionalization with folic acid reduced oxidative stress in rats. • Dysprosium doping does not affect the crystalline structure of hydroxyapatite. • Dysprosium doped particles are visible in fluorescent microscope. • Dysprosium doped particles act as MRI contrast agents

Development of Mucoadhesive Nanoparticulate System of Ebastine ...

African Journals Online (AJOL)

Purpose: To prepare and evaluate mucoadhesive nanoparticulate system of ebastine for nasal .... tripolyphosphate solution drop by drop to 3 ml of ... at an accelerating voltage of 20 KV before ..... i.e., around 1.0, then the size distribution of.

Synthesis of chitosan/hydroxyapatite membranes coated with hydroxycarbonate apatite for guided tissue regeneration purposes

Energy Technology Data Exchange (ETDEWEB)

Fraga, Alexandre Felix [Federal University of Sao Carlos, Department of Materials Engineering, DEMa, UFSCar, Sao Carlos, SP (Brazil); Almeida Filho, Edson de, E-mail: edsonafilho@yahoo.com.br [University Estadual Paulista, Department of Physical Chemistry - IQ, Araraquara, SP (Brazil); Silva Rigo, Eliana Cristina da [University of Sao Paulo, Department of Basic Science - FZEA-ZAB, Pirassununga, SP (Brazil); Ortega Boschi, Anselmo [Federal University of Sao Carlos, Department of Materials Engineering, DEMa, UFSCar, Sao Carlos, SP (Brazil)

2011-02-15

Chitosan, which is a non-toxic, biodegradable and biocompatible biopolymer, has been widely researched for several applications in the field of biomaterials. Calcium phosphate ceramics stand out among the so-called bioceramics for their absence of local or systemic toxicity, their non-response to foreign bodies or inflammations, and their apparent ability to bond to the host tissue. Hydroxyapatite (HA) is one of the most important bioceramics because it is the main component of the mineral phase of bone. The aim of this work was to produce chitosan membranes coated with hydroxyapatite using the modified biomimetic method. Membranes were synthesized from a solution containing 2% of chitosan in acetic acid (weight/volume) via the solvent evaporation method. Specimens were immersed in a sodium silicate solution and then in a 1.5 SBF (simulated body fluid) solution. The crystallinity of the HA formed over the membranes was correlated to the use of the nucleation agent (the sodium silicate solution itself). Coated membranes were characterized by means of scanning electron microscopy - SEM, X-ray diffraction - XRD, and Fourier transform infrared spectroscopy - FTIR. The results indicate a homogeneous coating covering the entire surface of the membrane and the production of a semi-crystalline hydroxyapatite layer similar to the mineral phase of human bone.

Study of mixed Ca-Zn hydroxyapatite surface modified by lactic acid

Science.gov (United States)

Turki, Thouraya; Aissa, Abdallah; Bac, Christophe Goze; Rachdi, Férid; Debbabi, Mongi

2012-07-01

The new hybrid inorganic-organic composites, Ca(10-x)Znx(PO4)6(OH)2-lactic acid, at different amounts of zinc and lactic acid were prepared by dissolution of the organic compound in an hydroxyapatite suspension. They were characterized by XRD, IR, MAS NMR (13C and 1H) and chemical analysis. The crystallinity was slightly affected by the presence of organic fragments. IR and (13C and 1H) MAS NMR measurements indicate that the carboxylic groups of the acid interact with calcium and zinc ions of hydroxyapatite surface. Chemical analysis displays that zinc promotes the acid grafting. A mechanism of surface modification is proposed based on the obtained results.

Study of mixed Ca-Zn hydroxyapatite surface modified by lactic acid

International Nuclear Information System (INIS)

Turki, Thouraya; Aissa, Abdallah; Bac, Christophe Goze; Rachdi, Férid; Debbabi, Mongi

2012-01-01

The new hybrid inorganic-organic composites, Ca (10-x) Zn x (PO 4 ) 6 (OH) 2 -lactic acid, at different amounts of zinc and lactic acid were prepared by dissolution of the organic compound in an hydroxyapatite suspension. They were characterized by XRD, IR, MAS NMR ( 13 C and 1 H) and chemical analysis. The crystallinity was slightly affected by the presence of organic fragments. IR and ( 13 C and 1 H) MAS NMR measurements indicate that the carboxylic groups of the acid interact with calcium and zinc ions of hydroxyapatite surface. Chemical analysis displays that zinc promotes the acid grafting. A mechanism of surface modification is proposed based on the obtained results.

Determination of Microstructural Parameters of Nanocrystalline Hydroxyapatite Prepared by Mechanical Alloying Method

Science.gov (United States)

Joughehdoust, Sedigheh; Manafi, Sahebali

2011-12-01

Hydroxyapatite [HA, Ca10(PO4)6(OH)2] is chemically similar to the mineral component of bones and hard tissues. HA can support bone ingrowth and osseointegration when used in orthopaedic, dental and maxillofacial applications. In this research, HA nanostructure was synthesized by mechanical alloying method. Phase development, particle size and morphology of HA were investigated by X-ray diffraction (XRD) pattern, zetasizer instrument, scanning electron microscopy (SEM), respectively. XRD pattern has been used to determination of the microstructural parameters (crystallite size, lattice parameters and crystallinity percent) by Williamson-Hall equation, Nelson-Riley method and calculating the areas under the peaks, respectively. The crystallite size and particle size of HA powders were in nanometric scales. SEM images showed that some parts of HA particles have agglomerates. The ratio of lattice parameters of synthetic hydroxyapatite (c/a = 0.73) was determined in this study is the same as natural hydroxyapatite structure.

Synthesis and Characterization of Nano-Hydroxyapatite/mPEG-b-PCL Composite Coating on Nitinol Alloy

Directory of Open Access Journals (Sweden)

Mohamadreza Etminanfar

2017-12-01

Full Text Available In this study the bioactivity of hydroxyapatite/poly(ε-caprolactone–poly(ethylene glycol bilayer coatings on Nitinol superelastic alloy was investigated. The surface of Nitinol alloy was activated by a thermo-chemical treatment and hydroxyapatite coating was electrodeposited on the alloy, followed by applying the polymer coating. The surface morphology of coatings was studied using FE-SEM and SEM. The data revealed that the hydroxyapatite coating is composed of one-dimensional nano sized flakes and the polymer coating is uniformly covered the sublayer. Also, High resolution TEM studies on the hydroxyapatite samples revealed that each flake contains nano-crystalline grains with a diameter of about 15 nm. The hydroxyapatite monolayer coating was rapidly covered by calcium phosphate crystals (Ca/P=1.7 after immersion in simulated body fluid confirming the bioactivity of the nanostructured flakes. However, the flakes were weak against applied external forces because of their ultra-fine thickness. Scratch test was applied on hydroxyapatite/polymer coating to evaluate delamination of the coating from substrate. It was shown that, the polymer coating has a great influence on toughening the hydroxyapatite coating. To assess the degradation effect of the polymer layer on hydroxyapatite coating, samples were immersed in phosphate-buffered saline at 37 ᵒC. SEM studies on the samples revealed that the beneath layer of hydroxyapatite appears after 72 h without any visible change in morphology. It seems that, application of a biodegradable polymer film on the nanostructured hydroxyapatite coating is a good way to support the coating during implantation processes

Electrocatalytic glucose oxidation at gold and gold-carbon nanoparticulate film prepared from oppositely charged nanoparticles

International Nuclear Information System (INIS)

Karczmarczyk, Aleksandra; Celebanska, Anna; Nogala, Wojciech; Sashuk, Volodymyr; Chernyaeva, Olga; Opallo, Marcin

2014-01-01

Graphical abstract: - Highlights: • Gold nanoparticulate film electrodes were prepared by layer-by-layer method from oppositely charged nanoparticles. • Positively charged nanoparticles play dominant role in glucose oxidation in alkaline solution. • Gold and gold-carbon nanoparticulate film electrodes exhibit similar glucose oxidation current and onset potential. - Abstract: Electrocatalytic oxidation of glucose was studied at nanoparticulate gold and gold-carbon film electrodes. These electrodes were prepared by a layer-by-layer method without application of any linker molecules. Gold nanoparticles were stabilized by undecane thiols functionalized by trimethyl ammonium or carboxylate groups, whereas the carbon nanoparticles were covered by phenylsulfonate functionalities. The gold nanoparticulate electrodes were characterized by UV-vis and XPS spectroscopy, atomic force microscopy and voltammetry, before and after heat-treatment. Heat-treatment facilitates the aggregation of the nanoparticles and affects the structure of the film. The comparison of the results obtained with film electrodes prepared from gold nanoparticles with the same charge and with gold-carbon nanoparticulate electrodes, proved that positively charged nanoparticles are responsible for the high electrocatalytic activity, whereas negatively charged ones act rather as a linker of the film

A comparative study of hydroxyapatite nanoparticles synthesized by different routes

OpenAIRE

Paz, Adrian; Guadarrama, Dainelys; López, Mónica; E. González, Jesús; Brizuela, Nayrim; Aragón, Javier

2012-01-01

In this study, bioactive hydroxyapatite nanoparticles were prepared by two different methods: wet chemical precipitation and biomimetic precipitation. The aim was to evaluate the morphology, particle-size, crystallinity and phases of the powders obtained by traditional wet chemical precipitation and the novel biomimetic precipitation using a supersaturated calcium solution. The nanoparticles were investigated by transmission electron microscopy, Fourier transform infrared spectroscopy and X-r...

On the compressibility of TiC in microcrystalline and nanoparticulate form

International Nuclear Information System (INIS)

Gu, Q F; Krauss, G; Steurer, W; Gramm, F

2008-01-01

The compressibility of TiC in microcrystalline and nanoparticulate (30-50 nm) form was studied by in situ high-pressure synchrotron radiation x-ray diffraction measurements up to 53.7 GPa using a diamond anvil cell. Both materials are structurally stable within the framework of the experiments applying quasihydrostatic pressure conditions. Under nonhydrostatic pressure conditions, the lattice of microcrystalline TiC is rhombohedrally distorted. Comparable values for the bulk modulus were found for both materials, i.e. K 0 = 254(7) GPa, K' = 4.8(4) for microcrystalline TiC and K 0 = 276(14) GPa, K' = 3.5(8) for nanoparticulate TiC, respectively. High-resolution transmission electron microscopy investigations revealed a nearly single-domain microstructure of the nanoparticles. The microstructure and size of the nanoparticles, making a size-induced effect on the mechanical properties negligible, explain well the observed similarity of the mechanical properties of microcrystalline and nanoparticulate TiC.

Synthesis of hydroxyapatite and structural refinement by X-ray diffraction; Sintese da hidroxiapatita e refinamento estrutural por difracao de raios-X

Energy Technology Data Exchange (ETDEWEB)

Araujo, Jorge Correa de [Universidade do Estado do Rio de Janeiro (UERJ), Sao Goncalo, RJ (Brazil). Faculdade de Formacao de Professores; Sena, Lidia [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (INMETRO), Duque de Caxias, RJ (Brazil). Div. de Metrologia de Materiais; Bastos, Ivan Napoleao [Universidade do Estado do Rio de Janeiro (UERJ), Nova Friburgo, RJ (Brazil). Inst. Politecnico]. E-mail: jcaraujo@iprj.uerj.br; Soares, Gloria Dulce de Almeida [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil)

2007-07-01

A sample of hydroxyapatite was synthesized and its crystalline structure was analyzed by X-ray diffraction by means of the Rietveld method. Two functions were used to fit the peak profiles, modified Voigt (TCHZ) and Pearson VII. The occupational factors and lattice parameters obtained by both models show that the sample does not contain relevant cationic substitutions. The interatomic distances from Ca1 to oxygens O1, O2 and O3 were adequate for a pure hydroxyapatite without defect at site Ca1. Besides, the use of multiple lines in planes (300) and (002) associated with the model Pearson VII resulted in good agreement with the TCHZ model with respect to the size-strain effects with an ellipsoidal shape of crystallites. In conclusion, the procedures adopted in the synthesis of hydroxyapatite produced a pure and crystalline material. The experimental results of transmission electron microscopy confirmed the predicted shape of crystals. (author)

Biogenic Hydroxyapatite: A New Material for the Preservation and Restoration of the Built Environment.

Science.gov (United States)

Turner, Ronald J; Renshaw, Joanna C; Hamilton, Andrea

2017-09-20

Ordinary Portland cement (OPC) is by weight the world's most produced man-made material and is used in a variety of applications in environments ranging from buildings, to nuclear wasteforms, and within the human body. In this paper, we present for the first time the direct deposition of biogenic hydroxyapatite onto the surface of OPC in a synergistic process which uses the composition of the cement substrate. This hydroxyapatite is very similar to that found in nature, having a similar crystallite size, iron and carbonate substitution, and a semi-crystalline structure. Hydroxyapatites with such a structure are known to be mechanically stronger and more biocompatible than synthetic or biomimetic hydroxyapatites. The formation of this biogenic hydroxyapatite coating therefore has significance in a range of contexts. In medicine, hydroxyapatite coatings are linked to improved biocompatibility of ceramic implant materials. In the built environment, hydroxyapatite coatings have been proposed for the consolidation and protection of sculptural materials such as marble and limestone, with biogenic hydroxyapatites having reduced solubility compared to synthetic apatites. Hydroxyapatites have also been established as effective for the adsorption and remediation of environmental contaminants such as radionuclides and heavy metals. We identify that in addition to providing a biofilm scaffold for nucleation, the metabolic activity of Pseudomonas fluorescens increases the pH of the growth medium to a suitable level for hydroxyapatite formation. The generated ammonia reacts with phosphate in the growth medium, producing ammonium phosphates which are a precursor to the formation of hydroxyapatite under conditions of ambient temperature and pressure. Subsequently, this biogenic deposition process takes place in a simple reaction system under mild chemical conditions and is cheap and easy to apply to fragile biological or architectural surfaces.

Novel Effects of Nanoparticulate Delivery of Zinc on Growth, Productivity, and Zinc Biofortification in Maize (Zea mays L.).

Science.gov (United States)

Subbaiah, Layam Venkata; Prasad, Tollamadugu Naga Venkata Krishna Vara; Krishna, Thimmavajjula Giridhara; Sudhakar, Palagiri; Reddy, Balam Ravindra; Pradeep, Thalappil

2016-05-18

In the present investigation, nanoscale zinc oxide particulates (ZnO-nanoparticulates) were prepared using a modified oxalate decomposition method. Prepared ZnO-nanoparticulates (mean size = 25 nm) were characterized using techniques such as transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), and zeta potential analyzer. Different concentrations (50, 100, 200, 400, 600, 800, 1000, 1500, and 2000 ppm) of ZnO-nanoparticulates were examined to reveal their effects on maize crop on overall growth and translocation of zinc along with bulk ZnSO4 and control. Highest germination percentage (80%) and seedling vigor index (1923.20) were observed at 1500 ppm of ZnO-nanoparticulates. The yield was 42% more compared to control and 15% higher compared to 2000 ppm of ZnSO4. Higher accumulation of zinc (35.96 ppm) in grains was recorded with application of 100 ppm followed by 400 ppm (31.05 ppm) of ZnO-nanoparticulates. These results indicate that ZnO-nanoparticulates have significant effects on growth, yield, and zinc content of maize grains, which is an important feature in terms of human health.

Surface modification of calcium hydroxyapatite by grafting of etidronic acid

Science.gov (United States)

Othmani, Masseoud; Aissa, Abdallah; Bac, Christophe Goze; Rachdi, Férid; Debbabi, Mongi

2013-06-01

The surface of prepared calcium hydroxyapatite CaHAp has been modified by grafting the etidronic acid (ETD). For that purpose, CaHAp powders have been suspended in an aqueous etidronate solution with different concentrations. The obtained composites CaHAp-(ETD) were characterized by TEM and AFM techniques to determinate morphological properties and were also characterized by XRD, IR, NMR and chemical and thermal analysis to determinate their physico-chemical properties and essentially the nature of the interaction between the inorganic support and the grafted organic ETD. After reaction with ETD, XRD powder analysis shows that the apatitic structure remains unchanged with slight affectation of its crystallinity. The presence of etidronate fragment bounded to hydroxyapatite was confirmed by IR and solid-state NMR spectroscopy. TEM and AFM techniques indicate that the presence of etidronate changes the morphology of the particles. Basing on the obtained results, a reactional mechanism was proposed to explain the formation of covalent Casbnd Osbnd Porg bonds on the hydroxyapatite surface between the superficial hydroxyl groups (tbnd Casbnd OH) of the apatite and phosphonate group (Psbnd OH) of etidronate.

Synthesis of hydroxyapatite nanoparticles by a novel ultrasonic assisted with mixed hollow sphere template method

Science.gov (United States)

Gopi, D.; Indira, J.; Kavitha, L.; Sekar, M.; Mudali, U. Kamachi

Hydroxyapatite (HAP) is the main inorganic component of bone material and is widely used in various biomedical applications due to its excellent bioactivity and biocompatibility. In this paper, we have reported the synthesis of hydroxyapatite nanoparticles by a novel ultrasonic assisted mixed template directed method. In this method glycine-acrylic acid (GLY-AA) hollow spheres were used as an organic template which could be prepared by mixing of glycine with acrylic acid. The as-synthesized HAP nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and tunnelling electron microscope (TEM) to investigate the nature of bonding, crystallinity, size and shape. The thermal stability of as-synthesized nanoparticles was also investigated by the thermo gravimetric analysis (TGA). The effect of ultrasonic irradiation time on the crystallinity and size of the HAP nanoparticles in presence of glycine-acrylic acid hollow spheres template were investigated. From the inspection of the above results it is confirmed that the crystallinity and size of the HAP nanoparticles decrease with increasing ultrasonic irradiation time. Hence the proposed synthesis strategy provides a facile pathway to obtain nano sized HAP with high quality, suitable size and morphology.

Nanoparticulate hollow TiO2 fibers as light scatterers in dye-sensitized solar cells: layer-by-layer self-assembly parameters and mechanism.

Science.gov (United States)

Rahman, Masoud; Tajabadi, Fariba; Shooshtari, Leyla; Taghavinia, Nima

2011-04-04

Hollow structures show both light scattering and light trapping, which makes them promising for dye-sensitized solar cell (DSSC) applications. In this work, nanoparticulate hollow TiO(2) fibers are prepared by layer-by-layer (LbL) self-assembly deposition of TiO(2) nanoparticles on natural cellulose fibers as template, followed by thermal removal of the template. The effect of LbL parameters such as the type and molecular weight of polyelectrolyte, number of dip cycles, and the TiO(2) dispersion (amorphous or crystalline sol) are investigated. LbL deposition with weak polyelectrolytes (polyethylenimine, PEI) gives greater nanoparticle deposition yield compared to strong polyelectrolytes (poly(diallyldimethylammonium chloride), PDDA). Decreasing the molecular weight of the polyelectrolyte results in more deposition of nanoparticles in each dip cycle with narrower pore size distribution. Fibers prepared by the deposition of crystalline TiO(2) nanoparticles show higher surface area and higher pore volume than amorphous nanoparticles. Scattering coefficients and backscattering properties of fibers are investigated and compared with those of commercial P25 nanoparticles. Composite P25-fiber films are electrophoretically deposited and employed as the photoanode in DSSC. Photoelectrochemical measurements showed an increase of around 50% in conversion efficiency. By employing the intensity-modulated photovoltage and photocurrent spectroscopy methods, it is shown that the performance improvement due to addition of fibers is mostly due to the increase in light-harvesting efficiency. The high surface area due to the nanoparticulate structure and strong light harvesting due to the hollow structure make these fibers promising scatterers in DSSCs. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparative physical, chemical and biological assessment of simple and titanium-doped ovine dentine-derived hydroxyapatite coatings fabricated by pulsed laser deposition

Energy Technology Data Exchange (ETDEWEB)

Duta, L.; Mihailescu, N.; Popescu, A.C.; Luculescu, C.R. [National Institute for Lasers, Plasma and Radiation Physics, 077125 Magurele (Romania); Mihailescu, I.N., E-mail: ion.mihailescu@inflpr.ro [National Institute for Lasers, Plasma and Radiation Physics, 077125 Magurele (Romania); Çetin, G.; Gunduz, O. [Department of Bioengineering, Faculty of Engineering, Marmara University, 34722 Istanbul (Turkey); Oktar, F.N. [Department of Bioengineering, Faculty of Engineering, Marmara University, 34722 Istanbul (Turkey); Department of Medical Imaging Techniques, Vocational School of Health Services, Marmara University, 34668 Istanbul (Turkey); Nanotechnology and Biomaterials Application & Research Centre, Marmara University, 34722 Istanbul (Turkey); Popa, A.C. [National Institute of Materials Physics, 077125 Magurele (Romania); Army Centre for Medical Research, 010195 Bucharest (Romania); Kuncser, A.; Besleaga, C. [National Institute of Materials Physics, 077125 Magurele (Romania); Stan, G.E., E-mail: george_stan@infim.ro [National Institute of Materials Physics, 077125 Magurele (Romania)

2017-08-15

Highlights: • Pulsed laser deposition of Ti doped hydroxyapatite films of biological origin. • Downgrade of films’ crystallinity and increase of roughness induced by Ti doping. • Bonding strength values superior to minimum value imposed by ISO standards. • Excellent biocompatibility in hMSC cultures of Ti doped structures. • Ti doped hydroxyapatite films as feasible materials for implantology applications. - Abstract: We report on the synthesis by Pulsed Laser Deposition of simple and Ti doped hydroxyapatite thin films of biological (ovine dentine) origin. Detailed physical, chemical, mechanical and biological investigations were performed. Morphological examination of films showed a surface composed of spheroidal particulates, of micronic size. Compositional analyses pointed to the presence of typical natural doping elements of bone, along with a slight non-stoichiometry of the deposited films. Structural investigations proved the monophasic hydroxyapatite nature of both simple and Ti doped films. Ti doping of biological hydroxyapatite induced an overall downgrade of the films crystallinity together with an increase of the films roughness. It is to be emphasized that bonding strength values measured at film/Ti substrate interface were superior to the minimum value imposed by International Standards regulating the load-bearing implant coatings. In vitro tests on Ti doped structures, compared to simple ones, revealed excellent biocompatibility in human mesenchymal stem cell cultures, a higher proliferation rate and a good cytocompatibility. The obtained results aim to elucidate the overall positive role of Ti doping on the hydroxyapatite films performance, and demonstrate the possibility to use this novel type of coatings as feasible materials for future implantology applications.

Comparative physical, chemical and biological assessment of simple and titanium-doped ovine dentine-derived hydroxyapatite coatings fabricated by pulsed laser deposition

International Nuclear Information System (INIS)

Duta, L.; Mihailescu, N.; Popescu, A.C.; Luculescu, C.R.; Mihailescu, I.N.; Çetin, G.; Gunduz, O.; Oktar, F.N.; Popa, A.C.; Kuncser, A.; Besleaga, C.; Stan, G.E.

2017-01-01

Highlights: • Pulsed laser deposition of Ti doped hydroxyapatite films of biological origin. • Downgrade of films’ crystallinity and increase of roughness induced by Ti doping. • Bonding strength values superior to minimum value imposed by ISO standards. • Excellent biocompatibility in hMSC cultures of Ti doped structures. • Ti doped hydroxyapatite films as feasible materials for implantology applications. - Abstract: We report on the synthesis by Pulsed Laser Deposition of simple and Ti doped hydroxyapatite thin films of biological (ovine dentine) origin. Detailed physical, chemical, mechanical and biological investigations were performed. Morphological examination of films showed a surface composed of spheroidal particulates, of micronic size. Compositional analyses pointed to the presence of typical natural doping elements of bone, along with a slight non-stoichiometry of the deposited films. Structural investigations proved the monophasic hydroxyapatite nature of both simple and Ti doped films. Ti doping of biological hydroxyapatite induced an overall downgrade of the films crystallinity together with an increase of the films roughness. It is to be emphasized that bonding strength values measured at film/Ti substrate interface were superior to the minimum value imposed by International Standards regulating the load-bearing implant coatings. In vitro tests on Ti doped structures, compared to simple ones, revealed excellent biocompatibility in human mesenchymal stem cell cultures, a higher proliferation rate and a good cytocompatibility. The obtained results aim to elucidate the overall positive role of Ti doping on the hydroxyapatite films performance, and demonstrate the possibility to use this novel type of coatings as feasible materials for future implantology applications.

Surface modification of calcium-copper hydroxyapatites using polyaspartic acid

Science.gov (United States)

Othmani, Masseoud; Aissa, Abdallah; Bachoua, Hassen; Debbabi, Mongi

2013-01-01

Mixed calcium-copper hydroxyapatite (Ca-CuHAp), with general formula Ca(10-x)Cux(PO4)6(OH)2, where 0 ≤ x ≤ 0.75 was prepared in aqueous medium in the presence of different concentrations of poly-L-aspartic acid (PASP). XRD, IR, TG-DTA, TEM-EDX, AFM and chemical analyses were used to characterize the structure, morphology and composition of the products. All techniques show the formation of new hybrid compounds Ca-CuHAp-PASP. The presence of the grafting moiety on the apatitic material is more significant with increasing of copper amount and/or organic concentration in the starting solution. These increases lead to the affectation of apatite crystallinity. The IR spectroscopy shows the conservation of (Psbnd OH) band of (HPO4)2- groups, suggesting that PASP acid was interacted only with metallic cations of hydroxyapatite.

Hydroxyapatite-Functionalized Graphene: A New Hybrid Nanomaterial

Directory of Open Access Journals (Sweden)

C. Rodríguez-González

2014-01-01

Full Text Available Graphene oxide sheets (GO were functionalized with hydroxyapatite nanoparticles (nHAp through a simple and effective hydrothermal treatment and a novel physicochemical process. Microstructure and crystallinity were investigated by Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy, X-ray diffraction (XRD, ultraviolet-visible (UV-Vis absorption spectroscopy, and thermogravimetric analysis (TGA. Transmission electron microscopy (TEM and scanning electron microscopy (SEM were performed to characterize the morphology of the functionalized material. The resulting novel materials combine the biocompatibility of the nHAp with the strength and physical properties of the graphene.

Nanostructured hydroxyapatite powders produced by a flame-based technique

Energy Technology Data Exchange (ETDEWEB)

Trommer, R.M., E-mail: rafael_trommer@yahoo.com.br [Ceramic Materials Laboratory, av. Osvaldo Aranha 99/705, 90035190, Porto Alegre, RS (Brazil); Santos, L.A. [Biomaterials Laboratory, av. Bento Goncalves 9500, Campus do Vale Setor IV Predio 74 Sala 123, 91501970, Porto Alegre, RS (Brazil); Bergmann, C.P. [Ceramic Materials Laboratory, av. Osvaldo Aranha 99/705, 90035190, Porto Alegre, RS (Brazil)

2009-08-01

In this work we reported the production of hydroxyapatite (HA) powder, one of the most studied calcium phosphates in the bioceramics field, using a cost-effective apparatus, composed by three major components: the atomization device, the pilot and main flames and finally the powder collector system. Calcium acetate and ammonium phosphate, diluted in ethanol and water, were used as salts in the precursor solution. The Ca/P molar ratio in the precursor solution was 1.65, equivalent to biological hydroxyapatite. After its production and collection, HA powder was calcined at 600 deg. C for 2 h. X-ray diffraction analysis pointed to the formation of crystalline hydroxyapatite powders. Carbonate was identified in the powders by Fourier-transform infrared (FTIR) spectroscopy. Scanning electronic microscopy (SEM) showed that the powders were composed of spherical primary particles and secondary aggregates, with the morphology unchanged after calcination. By transmission electronic microscopy (TEM), it was observed that the crystallite size of the primary particles was 24.8 {+-} 5.8 nm, for the calcined powder. The specific surface area was 15.03 {+-} 6.4 and 26.50 {+-} 7.6 m{sup 2}/g, for the as-synthetized and calcined powder respectively.

Synthesis of antimicrobial silver/hydroxyapatite nanocomposite by gamma irradiation

International Nuclear Information System (INIS)

Akhavan, A.; Sheikh, N.; Khoylou, F.; Naimian, F.; Ataeivarjovi, E.

2014-01-01

Silver nanoparticles (AgNPs) were synthesized through γ-irradiation reduction of silver ions into hydroxyapatite as a solid support. The formation of AgNPs incorporated in the hydroxyapatite composite was studied as a function of γ-irradiation doses. The X-ray diffraction and transmission electron microscopy (TEM) measurements showed the fabrication of face-centered cubic AgNPs with a mean diameter of about 39 nm at 20 kGy absorbed dose. When the absorbed dose increases from 20 to 40 kGy the size of AgNPs particles partially increases, while with increasing absorbed dose from 40 to 60 kGy the particle diameters decreases. In addition, the results of XRD analysis indicated that increasing of γ-irradiation doses from 20 to 40 kGy enhances the concentration of AgNPs, without inducing significant changes in degree of HA crystallinity. The antibacterial test study of samples against Escherichia coli indicated a significant enhancement in the antibacterial property of Ag/HA nanocomposites. - Highlights: • Silver/hydroxyapatite nanocomposites are synthesized through γ-irradiation method. • Ag/HA nanocomposites have good antibacterial properties. • Fabricated pure nanocomposites are suitable for medical and dental applications

Vibrational algorithms for quantitative crystallographic analyses of hydroxyapatite-based biomaterials: I, theoretical foundations.

Science.gov (United States)

Pezzotti, Giuseppe; Zhu, Wenliang; Boffelli, Marco; Adachi, Tetsuya; Ichioka, Hiroaki; Yamamoto, Toshiro; Marunaka, Yoshinori; Kanamura, Narisato

2015-05-01

The Raman spectroscopic method has quantitatively been applied to the analysis of local crystallographic orientation in both single-crystal hydroxyapatite and human teeth. Raman selection rules for all the vibrational modes of the hexagonal structure were expanded into explicit functions of Euler angles in space and six Raman tensor elements (RTE). A theoretical treatment has also been put forward according to the orientation distribution function (ODF) formalism, which allows one to resolve the statistical orientation patterns of the nm-sized hydroxyapatite crystallite comprised in the Raman microprobe. Close-form solutions could be obtained for the Euler angles and their statistical distributions resolved with respect to the direction of the average texture axis. Polarized Raman spectra from single-crystalline hydroxyapatite and textured polycrystalline (teeth enamel) samples were compared, and a validation of the proposed Raman method could be obtained through confirming the agreement between RTE values obtained from different samples.

Study of mixed Ca-Zn hydroxyapatite surface modified by lactic acid

Energy Technology Data Exchange (ETDEWEB)

Turki, Thouraya; Aissa, Abdallah [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia); Bac, Christophe Goze [Laboratoire Charles Coulomb, UMR 5221 CNRS/UM2, Universite Montpellier 2, Place E. Bataillon, 34095 Montpellier (France); Rachdi, Ferid, E-mail: Ferid.Rachdi@univ-montp2.fr [Laboratoire Charles Coulomb, UMR 5221 CNRS/UM2, Universite Montpellier 2, Place E. Bataillon, 34095 Montpellier (France); Debbabi, Mongi [Laboratoire de Physico-Chimie des Materiaux, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia)

2012-07-01

The new hybrid inorganic-organic composites, Ca{sub (10-x)}Zn{sub x}(PO{sub 4}){sub 6}(OH){sub 2}-lactic acid, at different amounts of zinc and lactic acid were prepared by dissolution of the organic compound in an hydroxyapatite suspension. They were characterized by XRD, IR, MAS NMR ({sup 13}C and {sup 1}H) and chemical analysis. The crystallinity was slightly affected by the presence of organic fragments. IR and ({sup 13}C and {sup 1}H) MAS NMR measurements indicate that the carboxylic groups of the acid interact with calcium and zinc ions of hydroxyapatite surface. Chemical analysis displays that zinc promotes the acid grafting. A mechanism of surface modification is proposed based on the obtained results.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

Science.gov (United States)

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of Mucoadhesive Nanoparticulate System of Ebastine ...

African Journals Online (AJOL)

Purpose: To prepare and evaluate mucoadhesive nanoparticulate system of ebastine for nasal drug delivery. Methods: The nanoparticles were prepared by ionic gelation method using drug-chitosan weight ratios 1:1, 1:2 and 1:3, and incorporating 0.5 or 0.7 % w/v sodium tripolyphosphate (STPP) and poloxamer 407.

Nanoscale crystallinity modulates cell proliferation on plasma sprayed surfaces

Energy Technology Data Exchange (ETDEWEB)

Smith, Alan M. [School of Applied Sciences, University of Huddersfield, Huddersfield HD1 3DH (United Kingdom); Paxton, Jennifer Z.; Hung, Yi-Pei; Hadley, Martin J.; Bowen, James; Williams, Richard L. [School of Chemical Engineering, University of Birmingham, Edgbaston, B15 2TT (United Kingdom); Grover, Liam M., E-mail: l.m.grover@bham.ac.uk [School of Chemical Engineering, University of Birmingham, Edgbaston, B15 2TT (United Kingdom)

2015-03-01

Calcium phosphate coatings have been applied to the surface of metallic prostheses to mediate hard and soft tissue attachment for more than 40 years. Most coatings are formed of high purity hydroxyapatite, and coating methods are often designed to produce highly crystalline surfaces. It is likely however, that coatings of lower crystallinity can facilitate more rapid tissue attachment since the surface will exhibit a higher specific surface area and will be considerably more reactive than a comparable highly crystalline surface. Here we test this hypothesis by growing a population of MC3T3 osteoblast-like cells on the surface of two types of hip prosthesis with similar composition, but with differing crystallinity. The surfaces with lower crystallinity facilitated more rapid cell attachment and increased proliferation rate, despite having a less heterogeneous surface topography. This work highlights that the influence of the crystallinity of HA at the nano-scale is dominant over macro-scale topography for cell adhesion and growth. Furthermore, crystallinity could be easily adjusted by without compromising coating purity. These findings could facilitate designing novel coated calcium phosphate surfaces that more rapidly bond tissue following implantation. - Highlights: • Crystallinity of HA at the nano-scale was dominant over macro-scale topography. • Lower crystallinity caused rapid cell attachment and proliferation rate. • Crystallinity could be easily adjusted by without compromising coating purity.

Nanoscale crystallinity modulates cell proliferation on plasma sprayed surfaces

International Nuclear Information System (INIS)

Smith, Alan M.; Paxton, Jennifer Z.; Hung, Yi-Pei; Hadley, Martin J.; Bowen, James; Williams, Richard L.; Grover, Liam M.

2015-01-01

Calcium phosphate coatings have been applied to the surface of metallic prostheses to mediate hard and soft tissue attachment for more than 40 years. Most coatings are formed of high purity hydroxyapatite, and coating methods are often designed to produce highly crystalline surfaces. It is likely however, that coatings of lower crystallinity can facilitate more rapid tissue attachment since the surface will exhibit a higher specific surface area and will be considerably more reactive than a comparable highly crystalline surface. Here we test this hypothesis by growing a population of MC3T3 osteoblast-like cells on the surface of two types of hip prosthesis with similar composition, but with differing crystallinity. The surfaces with lower crystallinity facilitated more rapid cell attachment and increased proliferation rate, despite having a less heterogeneous surface topography. This work highlights that the influence of the crystallinity of HA at the nano-scale is dominant over macro-scale topography for cell adhesion and growth. Furthermore, crystallinity could be easily adjusted by without compromising coating purity. These findings could facilitate designing novel coated calcium phosphate surfaces that more rapidly bond tissue following implantation. - Highlights: • Crystallinity of HA at the nano-scale was dominant over macro-scale topography. • Lower crystallinity caused rapid cell attachment and proliferation rate. • Crystallinity could be easily adjusted by without compromising coating purity

Isomorfic Substitutions of Calcium by Strontium in Calcium Hydroxyapatite

International Nuclear Information System (INIS)

Christensen, Hilbert

1962-12-01

By means of homogeneous precipitation it has been possible to synthesize crystalline solid solutions of calcium strontium hydroxyapatite from aqueous solutions. The lattice constants for the solid solutions were measured in the range Ca 9 Sr(PO 4 ) 6 (OH) 2 - CaSr 9 (PO 4 ) 6 (OH) 2 . The investigations show that the discrimination of strontium against calcium is considerably smaller than reported elsewhere (1). Strontium is preferentially built into the c-axis direction of the apatite lattice

Hybrid organic-inorganic materials based on hydroxyapatite structure

Energy Technology Data Exchange (ETDEWEB)

Moussa, Sana Ben; Bachouâ, Hassen [U.R. Matériaux et synthèse organique UR17ES31, Institut Préparatoire aux Etudes d’Ingénieur de Monastir, Université de Monastir, 5019 Monastir (Tunisia); Gruselle, Michel, E-mail: michel.gruselle@upmc.fr [Sorbonne Université, UPMC Univ Paris 06, CNRS, UMR 8232, Institut Parisien de Chimie Moléculaire, F-75005 Paris (France); Beaunier, Patricia [Sorbonne Université, UPMC Univ Paris 06, CNRS, UMR 7197, Laboratoire de Réactivité de Surface, F-75005 Paris (France); Flambard, Alexandrine [Sorbonne Université, UPMC Univ Paris 06, CNRS, UMR 8232, Institut Parisien de Chimie Moléculaire, F-75005 Paris (France); Badraoui, Béchir [U.R. Matériaux et synthèse organique UR17ES31, Institut Préparatoire aux Etudes d’Ingénieur de Monastir, Université de Monastir, 5019 Monastir (Tunisia)

2017-04-15

The present article details the formation of calcium hydroxyapatite synthesized by the hydrothermal way, in presence of glycine or sarcosine. The presence of these amino-acids during the synthetic processes reduces the crystalline growthing through the formation of hybrid organic-inorganic species The crystallite sizes are decreasing and the morphology is modified with the increase of the amino-acid concentration. - Graphical abstract: Formation of Ca carboxylate salt leading to the grafting of glycine and sarcosine on the Ca=Hap surface (R= H, CH3).

Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Agougui, H.; Aissa, A. [Laboratoire de Physico-Chimie des Materiaux, Faculte des sciences de Monastir, 5019 Monastir (Tunisia); Maggi, S. [CNR-IC Istituto di Cristallografia, via Amendola 122/O, 70126 Bari (Italy); Debbabi, M., E-mail: m.debbabi@yahoo.fr [Laboratoire de Physico-Chimie des Materiaux, Faculte des sciences de Monastir, 5019 Monastir (Tunisia)

2010-12-15

Calcium hydroxyapatite (CaHAp) was prepared in the presence of two alkylphosphonates, the tert-butyl phosphonic acid TBPOH and the 2-carboxyletylphosphonic acid 2-CEPA, by hydrothermal method at 120 deg. C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ({sup 1}H and {sup 31}P) spectroscopy and chemical analysis. X-ray powder diffraction patterns show that the incorporation of organic moieties induces a significant loss of the material crystallinity and a clear increase of the unit cell lattice parameter a as function of 2-CEPA grafting rate. The specific surface area (SSA) increases with increasing phosphonate amount especially for 2-CEPA. All techniques show the lower reactivity of TBPOH due to the steric effects of tert-butyl, whereas the 2-CEPA with a linear chain and double acidic functions is more reactive and can replace the OH{sup -} groups of the apatitic structure.

Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

International Nuclear Information System (INIS)

Agougui, H.; Aissa, A.; Maggi, S.; Debbabi, M.

2010-01-01

Calcium hydroxyapatite (CaHAp) was prepared in the presence of two alkylphosphonates, the tert-butyl phosphonic acid TBPOH and the 2-carboxyletylphosphonic acid 2-CEPA, by hydrothermal method at 120 deg. C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ( 1 H and 31 P) spectroscopy and chemical analysis. X-ray powder diffraction patterns show that the incorporation of organic moieties induces a significant loss of the material crystallinity and a clear increase of the unit cell lattice parameter a as function of 2-CEPA grafting rate. The specific surface area (SSA) increases with increasing phosphonate amount especially for 2-CEPA. All techniques show the lower reactivity of TBPOH due to the steric effects of tert-butyl, whereas the 2-CEPA with a linear chain and double acidic functions is more reactive and can replace the OH - groups of the apatitic structure.

Novel silk fibroin films prepared by formic acid/hydroxyapatite dissolution method

International Nuclear Information System (INIS)

Ming, Jinfa; Liu, Zhi; Bie, Shiyu; Zhang, Feng; Zuo, Baoqi

2014-01-01

Bombyx mori silk fibroin from the silkworm was firstly found to be soluble in formic acid/hydroxyapatite system. The rheological behavior of silk fibroin solution was significantly influenced by HAp contents in dissolved solution. At the same time, silk fibroin nanofibers were observed in dissolved solution with 103.6 ± 20.4 nm in diameter. Moreover, the structure behavior of SF films prepared by formic acid/hydroxyapatite dissolution method was examined. The secondary structure of silk fibroin films was attributed to silk II structure (β-sheet), indicating that the hydroxyapatite contents in dissolved solution were not significantly affected by the structure of silk fibroin. The X-ray diffraction results exhibited obviously hydroxyapatite crystalline nature existing in silk fibroin films; however, when the hydroxyapatite content was 5.0 wt.% in dissolved solution, some hydroxyapatite crystals were converted to calcium hydrogen phosphate dehydrate in silk fibroin dissolution process. This result was also confirmed by Fourier transform infrared analysis and DSC measurement. In addition, silk fibroin films prepared by this dissolution method had higher breaking strength and extension at break. Based on these analyses, an understanding of novel SF dissolution method may provide an additional tool for designing and synthesizing advanced materials with more complex structures, which should be helpful in different fields, including biomaterial applications. - Highlights: • SF fibers were firstly successfully dissolved in FA/HAp solution. • The rheological behavior of SF solution was significantly influenced by HAp contents. • SF nanofibrils were observed in FA/HAp solution with 103.6 ± 20.4 nm in diameter. • SF films prepared by FA/HAp dissolution method had higher mechanical properties

Novel silk fibroin films prepared by formic acid/hydroxyapatite dissolution method

Energy Technology Data Exchange (ETDEWEB)

Ming, Jinfa, E-mail: jinfa.ming@gmail.com [National Engineering Laboratory for Modern Silk, Soochow University, Suzhou 215123 (China); College of Textile and Clothing Engineering, Soochow University, Suzhou 215021 (China); Liu, Zhi; Bie, Shiyu [National Engineering Laboratory for Modern Silk, Soochow University, Suzhou 215123 (China); College of Textile and Clothing Engineering, Soochow University, Suzhou 215021 (China); Zhang, Feng [Jiangsu Province Key Laboratory of Stem Cell Research, Medical College, Soochow University, Suzhou 215006 (China); Zuo, Baoqi, E-mail: bqzuo@suda.edu.cn [National Engineering Laboratory for Modern Silk, Soochow University, Suzhou 215123 (China); College of Textile and Clothing Engineering, Soochow University, Suzhou 215021 (China)

2014-04-01

Bombyx mori silk fibroin from the silkworm was firstly found to be soluble in formic acid/hydroxyapatite system. The rheological behavior of silk fibroin solution was significantly influenced by HAp contents in dissolved solution. At the same time, silk fibroin nanofibers were observed in dissolved solution with 103.6 ± 20.4 nm in diameter. Moreover, the structure behavior of SF films prepared by formic acid/hydroxyapatite dissolution method was examined. The secondary structure of silk fibroin films was attributed to silk II structure (β-sheet), indicating that the hydroxyapatite contents in dissolved solution were not significantly affected by the structure of silk fibroin. The X-ray diffraction results exhibited obviously hydroxyapatite crystalline nature existing in silk fibroin films; however, when the hydroxyapatite content was 5.0 wt.% in dissolved solution, some hydroxyapatite crystals were converted to calcium hydrogen phosphate dehydrate in silk fibroin dissolution process. This result was also confirmed by Fourier transform infrared analysis and DSC measurement. In addition, silk fibroin films prepared by this dissolution method had higher breaking strength and extension at break. Based on these analyses, an understanding of novel SF dissolution method may provide an additional tool for designing and synthesizing advanced materials with more complex structures, which should be helpful in different fields, including biomaterial applications. - Highlights: • SF fibers were firstly successfully dissolved in FA/HAp solution. • The rheological behavior of SF solution was significantly influenced by HAp contents. • SF nanofibrils were observed in FA/HAp solution with 103.6 ± 20.4 nm in diameter. • SF films prepared by FA/HAp dissolution method had higher mechanical properties.

Preparation and structure of carbonated calcium hydroxyapatite substituted with heavy rare earth ions

Energy Technology Data Exchange (ETDEWEB)

Yasukawa, Akemi, E-mail: yasukawa@cc.hirosaki-u.ac.jp [School of Home Economics, Faculty of Education, Hirosaki University, 1-bunkyo, Hirosaki, Aomori 036-8560 (Japan); Kandori, Kazuhiko [School of Chemistry, Osaka University of Education, 4-698-1 Asahigaoka, Kashiwara, Osaka 582-8582 (Japan); Tanaka, Hidekazu [Department of Material Science, Faculty of Science and Engineering, Shimane University, 1060 Nishikawatsu, Matsue, Shimane 690-8504 (Japan); Gotoh, Keiko [Faculty of Human Life and Environment, Nara Women' s University, Kita-uoya-nishi, Nara 630-8506 (Japan)

2012-05-15

Highlights: Black-Right-Pointing-Pointer LnCaHap solid solution particles were prepared using five types of heavy rare earth ions by a precipitation method. Black-Right-Pointing-Pointer The length and the crystallinity of the LnCaHap particles first increased and then decreased with increasing Ln{sup 3+} contents. Black-Right-Pointing-Pointer A series of YCaHap solid solution particles formed with Y/(Y + Ca) = 0-0.10 were investigated using various methods in detail. -- Abstract: Calcium hydroxyapatite (CaHap) particles substituted five types of heavy rare earth ions (Ln: Y{sup 3+}, Gd{sup 3+}, Dy{sup 3+}, Er{sup 3+} and Yb{sup 3+}) were synthesized using a precipitation method and characterized using various means. These Ln ions strongly affected the crystal phases and the structures of the products. With increasing Ln/(Ln + Ca) in the starting solution ([X{sub Ln}]), the length and the crystallinity of the particles first increased and then decreased. The rare earth metal-calcium hydroxyapatite (LnCaHap) solid solution particles were obtained at [X{sub Y}] {<=} 0.10 for substituting Y system and at [X{sub Ln}] {<=} 0.01-0.03 for substituting the other Ln systems. LnPO{sub 4} was mixed with LnCaHap at higher [X{sub Ln}] for all Ln systems. A series of yttrium-calcium hydroxyapatite (YCaHap) solid solutions with [X{sub Y}] = 0-0.10 were investigated using XRD, TEM, ICP-AES, IR and TG-DTA in detail.

Preparation and structure of carbonated calcium hydroxyapatite substituted with heavy rare earth ions

International Nuclear Information System (INIS)

Yasukawa, Akemi; Kandori, Kazuhiko; Tanaka, Hidekazu; Gotoh, Keiko

2012-01-01

Highlights: ► LnCaHap solid solution particles were prepared using five types of heavy rare earth ions by a precipitation method. ► The length and the crystallinity of the LnCaHap particles first increased and then decreased with increasing Ln 3+ contents. ► A series of YCaHap solid solution particles formed with Y/(Y + Ca) = 0–0.10 were investigated using various methods in detail. -- Abstract: Calcium hydroxyapatite (CaHap) particles substituted five types of heavy rare earth ions (Ln: Y 3+ , Gd 3+ , Dy 3+ , Er 3+ and Yb 3+ ) were synthesized using a precipitation method and characterized using various means. These Ln ions strongly affected the crystal phases and the structures of the products. With increasing Ln/(Ln + Ca) in the starting solution ([X Ln ]), the length and the crystallinity of the particles first increased and then decreased. The rare earth metal-calcium hydroxyapatite (LnCaHap) solid solution particles were obtained at [X Y ] ≤ 0.10 for substituting Y system and at [X Ln ] ≤ 0.01–0.03 for substituting the other Ln systems. LnPO 4 was mixed with LnCaHap at higher [X Ln ] for all Ln systems. A series of yttrium-calcium hydroxyapatite (YCaHap) solid solutions with [X Y ] = 0–0.10 were investigated using XRD, TEM, ICP-AES, IR and TG–DTA in detail.

Novel synthesis strategy for composite hydrogel of collagen/hydroxyapatite-microsphere originating from conversion of CaCO3 templates.

Science.gov (United States)

Wei, Qingrong; Lu, Jian; Wang, Qiaoying; Fan, Hongsong; Zhang, Xingdong

2015-03-20

Inspired by coralline-derived hydroxyapatite, we designed a methodological route to synthesize carbonated-hydroxyapatite microspheres from the conversion of CaCO3 spherulite templates within a collagen matrix under mild conditions and thus constructed the composite hydrogel of collagen/hydroxyapatite-microspheres. Fourier transform infrared spectroscopy (FTIR) and x-ray diffraction (XRD) were employed to confirm the successful generation of the carbonated hydroxyapatite phase originating from CaCO3, and the ratios of calcium to phosphate were tracked over time. Variations in the weight portion of the components in the hybrid gels before and after the phase transformation of the CaCO3 templates were identified via thermogravimetric analysis (TGA). Scanning electron microscopy (SEM) shows these composite hydrogels have a unique multiscale microstructure consisting of a collagen nanofibril network and hydroxyapatite microspheres. The relationship between the hydroxyapatite nanocrystals and the collagen fibrils was revealed by transmission electron microscopy (TEM) in detail, and the selected area electron diffraction (SAED) pattern further confirmed the results of the XRD analyses which show the typical low crystallinity of the generated hydroxyapatite. This smart synthesis strategy achieved the simultaneous construction of microscale hydroxyapatite particles and collagen fibrillar hydrogel, and appears to provide a novel route to explore an advanced functional hydrogel materials with promising potentials for applications in bone tissue engineering and reconstruction medicine.

Arsenic sorption to nanoparticulate mackinawite (FeS): An examination of phosphate competition.

Science.gov (United States)

Niazi, Nabeel Khan; Burton, Edward D

2016-11-01

Nanoparticulate mackinawite (FeS) can be an important host-phase for arsenic (As) in sulfidic, subsurface environments. Although not previously investigated, phosphate (PO 4 3- ) may compete with As for available sorption sites on FeS, thereby enhancing As mobility in FeS-bearing soils, sediments and groundwater systems. In this study, we examine the effect of PO 4 3- on sorption of arsenate (As(V)) and arsenite (As(III)) to nanoparticulate FeS at pH 6, 7 and 9. Results show that PO 4 3- (at 0.01-1.0 mM P) did not significantly affect sorption of either As(V) or As(III) to nanoparticulate FeS at initial aqueous As concentrations ranging from 0.01 to 1.0 mM. At pH 9 and 7, sorption of both As(III) and As(V) to nanoparticulate FeS was similar, with distribution coefficient (K d ) values spanning 0.76-15 L g -1 (which corresponds to removal of 87-98% of initial aqueous As(III) and As(V) concentrations). Conversely, at pH 6, the sorption of As(III) was characterized by substantially higher K d values (6.3-93.4 L g -1 ) than those for As(V) (K d  = 0.21-0.96 L g -1 ). Arsenic K-edge X-ray absorption near edge structure (XANES) spectroscopy indicated that up to 52% of the added As(V) was reduced to As(III) in As(V) sorption experiments, as well as the formation of minor amounts of an As 2 S 3 -like species. In As(III) sorption experiments, XANES spectroscopy also demonstrated the formation of an As 2 S 3 -like species and the partial oxidation of As(III) to As(V) (despite the strictly O 2 -free experimental conditions). Overall, the XANES data indicate that As sorption to nanoparticulate FeS involves several redox transformations and various sorbed species, which display a complex dependency on pH and As loading but that are not influenced by the co-occurrence of PO 4 3- . This study shows that nanoparticulate FeS can help to immobilize As(III) and As(V) in sulfidic subsurface environments where As co-exists with PO 4 3- . Copyright © 2016 Elsevier Ltd. All

Critical ageing and chemistry of nanocrystalline hydroxyapatite sol-gel solutions

Energy Technology Data Exchange (ETDEWEB)

Chai, C.S.; Gross, K.A.; Kannangara, K.; Ben-Nissan, B. [University of Technology, Sydney, NSW (Australia). Department of Chemistry, Materials and Forensic Sciences; Hanley, L. [University of Illinois at Chicago, (United States). Department of Chemistry

1998-12-31

In previous work we have demonstrated that using alkoxide precursors, it is possible to produce crystalline hydroxyapatite coatings with potential uses in orthopaedic and dental applications. However, to produce monophasic hydroxyapatite coatings, sols must be aged for a minimum of 24 hours prior to deposition. {sup 31}P NMR has been used to analyse chemical changes occurring in the sol during the ageing process and have revealed that P-O-C bonds present in the precursor material are gradually replaced by P-O-Ca bonds with an accompanying change in oxidation state from P(III) to P(V). Thermal analysis was used to examine hydrolysed gels and showed that sols aged less than 24 hours contain unreacted calcium diethoxide which produces CaO upon heating. These findings have been confirmed by x-ray diffraction. Copyright (1998) Australasian Ceramic Society 16 refs., 4 figs.

Critical ageing and chemistry of nanocrystalline hydroxyapatite sol-gel solutions

International Nuclear Information System (INIS)

Chai, C.S.; Gross, K.A.; Kannangara, K.; Ben-Nissan, B.; Hanley, L.

1998-01-01

In previous work we have demonstrated that using alkoxide precursors, it is possible to produce crystalline hydroxyapatite coatings with potential uses in orthopaedic and dental applications. However, to produce monophasic hydroxyapatite coatings, sols must be aged for a minimum of 24 hours prior to deposition. 31 P NMR has been used to analyse chemical changes occurring in the sol during the ageing process and have revealed that P-O-C bonds present in the precursor material are gradually replaced by P-O-Ca bonds with an accompanying change in oxidation state from P(III) to P(V). Thermal analysis was used to examine hydrolysed gels and showed that sols aged less than 24 hours contain unreacted calcium diethoxide which produces CaO upon heating. These findings have been confirmed by x-ray diffraction. Copyright (1998) Australasian Ceramic Society

On the mechanism of nanoparticulate CeO{sub 2} toxicity to freshwater algae

Energy Technology Data Exchange (ETDEWEB)

Angel, Brad M., E-mail: Brad.Angel@csiro.au [Centre for Environmental Contaminants Research, CSIRO Land and Water Flagship, Locked Bag 2007, Kirrawee, NSW 2232 (Australia); Vallotton, Pascal [Digital Productivity Flagship, CSIRO, North Ryde, NSW 1670 (Australia); Apte, Simon C. [Centre for Environmental Contaminants Research, CSIRO Land and Water Flagship, Locked Bag 2007, Kirrawee, NSW 2232 (Australia)

2015-11-15

Highlights: • Nanoparticulate CeO{sub 2} less toxic than micron-sized CeO{sub 2}. • UV light filters prevented ROS generation by CeO{sub 2}. • ROS not toxic mechanism: CeO{sub 2} toxicity was similar in presence and absence of ROS. • Strong sorption of nanoparticulate CeO{sub 2} to Pseudokirchneriella subcapitata in synthetic fresh water. • CeO{sub 2} sorption to cells was prevented and toxicity mitigated in the presence of DOC. - Abstract: The factors affecting the chronic (72-h) toxicity of three nanoparticulate (10–34 nm) and one micron-sized form of CeO{sub 2} to the green alga, Pseudokirchneriella subcapitata were investigated. To characterise transformations in solution, hydrodynamic diameters (HDD) were measured by dynamic light scatter, zeta potential values by electrophoretic mobility, and dissolution by equilibrium dialysis. The protective effects of humic and fulvic dissolved organic carbon (DOC) on toxicity were also assessed. To investigate the mechanisms of algal toxicity, the CytoViva hyperspectral imaging system was used to visualise algal–CeO{sub 2} interactions in the presence and absence of DOC, and the role of reactive oxygen species (ROS) was investigated by ‘switching off’ ROS production using UV-filtered lighting conditions. The nanoparticulate CeO{sub 2} immediately aggregated in solution to HDDs measured in the range 113–193 nm, whereas the HDD and zeta potential values were significantly lower in the presence of DOC. Negligible CeO{sub 2} dissolution over the time course of the bioassay ruled out potential toxicity from dissolved cerium. The nanoparticulate CeO{sub 2} concentration that caused 50% inhibition of algal growth rate (IC50) was in the range 7.6–28 mg/L compared with 59 mg/L for micron-sized ceria, indicating that smaller particles were more toxic. The presence of DOC mitigated toxicity, with IC50s increasing to greater than 100 mg/L. Significant ROS were generated in the nanoparticulate CeO{sub 2

Synthesis of hydroxyapatite nanoparticles by a novel ultrasonic assisted with mixed hollow sphere template method.

Science.gov (United States)

Gopi, D; Indira, J; Kavitha, L; Sekar, M; Mudali, U Kamachi

2012-07-01

Hydroxyapatite (HAP) is the main inorganic component of bone material and is widely used in various biomedical applications due to its excellent bioactivity and biocompatibility. In this paper, we have reported the synthesis of hydroxyapatite nanoparticles by a novel ultrasonic assisted mixed template directed method. In this method glycine-acrylic acid (GLY-AA) hollow spheres were used as an organic template which could be prepared by mixing of glycine with acrylic acid. The as-synthesized HAP nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and tunnelling electron microscope (TEM) to investigate the nature of bonding, crystallinity, size and shape. The thermal stability of as-synthesized nanoparticles was also investigated by the thermo gravimetric analysis (TGA). The effect of ultrasonic irradiation time on the crystallinity and size of the HAP nanoparticles in presence of glycine-acrylic acid hollow spheres template were investigated. From the inspection of the above results it is confirmed that the crystallinity and size of the HAP nanoparticles decrease with increasing ultrasonic irradiation time. Hence the proposed synthesis strategy provides a facile pathway to obtain nano sized HAP with high quality, suitable size and morphology. Copyright © 2012 Elsevier B.V. All rights reserved.

Use of micrometric latex beads to improve the porosity of hydroxyapatite obtained by chemical coprecipitation method

Science.gov (United States)

Webler, G. D.; Rodrigues, W. C.; Silva, A. E. S.; Silva, A. O. S.; Fonseca, E. J. S.; Degenhardt, M. F. S.; Oliveira, C. L. P.; Otubo, L.; Barros Filho, D. A.

2018-04-01

Hydroxyapatite is one of the most important biomaterials whose application mainly extends to implants and drug delivery. This work will discuss the changes in the pore size distribution of hydroxyapatite when there are latex beads present during the synthesis. These changes were monitored using different techniques: small angle X-ray scattering, X-ray diffraction, thermal gravimetrical analysis, N2 adsorption, scanning and transmission electron microscopy. Latex beads and hydroxyapatite form a single nanocomposite with well-distinguished inorganic and organic phases. Latex bead removal in the temperature range of 300-600 °C did not modify the original crystalline structure of hydroxyapatite. However, the latex beads favored an increase in the adsorption capacity of mesopores at temperatures higher than their glassy transition (Tg). The main result of this research work consists on the increase of surface area and pore size distribution obtained after the removal of latex beads template. Latex beads have been used in a different approach changing the porosity of hydroxyapatite scaffolds not only introducing new routes for cell integration but also broadening the pore size distribution which can result in a more high efficiency for drug release in living cells.

Synthesis of nano-hydroxyapatite (nHA) from waste mussel shells using a rapid microwave method

Energy Technology Data Exchange (ETDEWEB)

Shavandi, Amin, E-mail: amin.shavandi@postgrad.otago.ac.nz [Department of Food Sciences, University of Otago, Dunedin (New Zealand); Bekhit, Alaa El-Din A. [Department of Food Sciences, University of Otago, Dunedin (New Zealand); Ali, Azam [Department of Applied Sciences, University of Otago, Dunedin (New Zealand); Sun, Zhifa [Department of Physics, University of Otago, Dunedin (New Zealand)

2015-01-15

Nano-crystalline hydroxyapatite (HA, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}) was produced from waste mussel shells using a rapid microwave irradiation method. Mussel shells were converted to rod like nano-crystalline HA particles of 30–70 nm long using 0.1 M EDTA as a chelating agent for 30 min after an appropriate pre-treatment and an irradiation step in a microwave with a power of 1.1 kW. The produced HA was characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), thermo gravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR) and inductively coupled plasma mass spectrometry (ICP-MS) to determine the morphology, particle size, crystal phases, elemental composition and thermal behaviour. Furthermore, to benchmark the synthesized HA obtained from mussel shells, it was compared with a commercially pure HA (Sigma–Aldrich). The thermal analysis showed that the synthesized HA has remarkable heat stability at 1000 °C, and the XRD and FTIR results showed a high purity of the synthesized HA powders. Compared to the conventional hydrothermal treatment, microwave-assisted method has the advantages of an increased rate of HA formation. The obtained HA have potential engineering applications as materials for bone-tissues. - Highlights: • Waste mussel shells were successfully converted to nano sized hydroxyapatite. • Microwave-assisted technique accelerated the conversion process. • The physicochemical properties of the produced hydroxyapatite are reported. • The prepared hydroxyapatite has nano sized particles of less than 100 nm.

Lability of nanoparticulate metal complexes in electrochemical speciation analysis

DEFF Research Database (Denmark)

van Leeuwen, Herman P.; Town, Raewyn M.

2016-01-01

Lability concepts are elaborated for metal complexes with soft (3D) and hard (2D) aqueous nanoparticles. In the presence of a non-equilibrium sensor, e.g. a voltammetric electrode, the notion of lability for nanoparticulate metal complexes, M-NP, reflects the ability of the M-NP to maintain...... equilibrium with the reduced concentration of the electroactive free M2+ in its diffusion layer. Since the metal ion binding sites are confined to the NP body, the conventional reaction layer in the form of a layer adjacent to the electrode surface is immaterial. Instead an intraparticulate reaction zone may...... of the electrochemical technique is crucial in the lability towards the electrode surface. In contrast, for nanoparticulate complexes it is the dynamics of the exchange of the electroactive metal ion with the surrounding medium that governs the effective lability towards the electrode surface....

Surface roughness of microparticulated and nanoparticulated composites after finishing and polishing procedures

Directory of Open Access Journals (Sweden)

Rosemary Arai Sadami Shinkai

Full Text Available Objective: To evaluated the surface roughness of one microparticulate resin composite Durafill (Heraeus Kulzer Weihrheim, Germany andfour nanoparticulate resins 4 Seasons (Ivoclar Vivadent, Schaan, Liechtenstein Esthet x (Dentsply, Milford, DE, USA, Point 4 and Supreme (3M-ESPE, Dental Products,St. Paul, MN, USA. Methods: After finishing with a diamond bur point (F, and polishing with silicone points of gray, green and pink color Politipit (Ivoclar Vivadent,Schaan, Liechtenstein, four stages of completion were performed, simulating one of finishing and three of polishing a resin restoration. Ten samples of each composite resin were measured for surface roughness with surface profilometer (Mitutoyo Corporation, Tokyo, Japan after each of finishing and polishing sequence.Results: The results showed that nanoparticulate and microparticulate resins presented a significant difference in the surface roughness values, in all finishing and polishing steps. Conclusion: Of the the nanoparticulate resins 4 Seasons (Ivoclar Vivadent, Schaan, Liechtenstein, Point 4 (Kerr CO, Orange, CA, USA, and also microparticulate Durafill (Heraeus Kulzer Weihrheim, Germany presented significantly lower surface roughness values after completing all the finishing and polishing stages.

Isomorfic Substitutions of Calcium by Strontium in Calcium Hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Christensen, Hilbert

1962-12-15

By means of homogeneous precipitation it has been possible to synthesize crystalline solid solutions of calcium strontium hydroxyapatite from aqueous solutions. The lattice constants for the solid solutions were measured in the range Ca{sub 9}Sr(PO{sub 4}){sub 6}(OH){sub 2} - CaSr{sub 9}(PO{sub 4}){sub 6}(OH){sub 2}. The investigations show that the discrimination of strontium against calcium is considerably smaller than reported elsewhere (1). Strontium is preferentially built into the c-axis direction of the apatite lattice.

Influence of hydroxyapatite granule size, porosity, and crystallinity on tissue reaction in vivo. Part A: synthesis, characterization of the materials, and SEM analysis.

Science.gov (United States)

Maté Sánchez de Val, José E; Calvo-Guirado, José L; Gómez-Moreno, Gerardo; Pérez-Albacete Martínez, Carlos; Mazón, Patricia; De Aza, Piedad N

2016-11-01

The aim of this study was the synthesis and analysis of the tissue reaction to three different Hydroxyapatite (HA)-based bone substitute materials differing only in granule size, porosity, and crystallinity through an animal experimental model at 60 days. Three different HA-based biomaterials were synthesized and characterized by X-ray diffraction, SEM, and EDS analysis, the resultant product was ground in three particle sizes: Group I (2000-4000 μm), Group II (1000-2000 μm), and Group III (600-1000 μm). Critical size defects were created in both tibias of 15 rabbits. Four defects per rabbit for a total of 60 defects were grafted with the synthesized materials as follows: Group I (15 defects), Group II (15 defects), Group III (15 defects), and empty (15 defects control). After animals sacrifice at 60 days samples were obtained and processed for SEM and EDS evaluation of Ca/P ratios, elemental mapping was performed to determine the chemical degradation process and changes to medullary composition in all the four study groups. The tendency for the density was to increase with the increasing annealing temperature; in this way it was possible to observe that the sample that shows highest crystallinity and crystal size corresponding to that of group I. The SEM morphological examination showed that group III implant showed numerous resorption regions, group II implant presented an average resorption rate of all the implants. The group I displayed smoother surface features, in comparison with the other two implants. The data from this study show that changing the size, porosity, and crystallinity of one HA-based bone substitute material can influence the integration of the biomaterials within the implantation site and the new bone formation. © 2015 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Structural and mechanical properties of hydroxyapatite coatings formed by ion-beam assisted deposition

Science.gov (United States)

Zykova, A.; Safonov, V.; Dudin, S.; Yakovin, S.; Donkov, N.; Ghaemi, M. H.; Szkodo, M.; Antoszkiewicz, M.; Szyfelbain, M.; Czaban, A.

2018-03-01

The ion-beam assisted deposition (IBAD) is an advanced method capable of producing crystalline coatings at low temperatures. We determined the characteristics of hydroxyapatite Ca10(PO4)6(OH)2 target and coatings formed by IBAD using X-ray photoemission spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and energy dispersive X-ray (EDX). The composition of the coatings’ cross-section and surface was close to those of the target. The XPS spectra showed that the binding energy values of Ca (2p1/2, 2p3/2), P (2p3/2), and O 1s levels are related to the hydroxyapatite phase. The coatings demonstrate an optimal H/E ratio, and a good resistance to scratch tests.

Structure–property relationships of iron–hydroxyapatite ceramic matrix nanocomposite fabricated using mechanosynthesis method

Energy Technology Data Exchange (ETDEWEB)

Nordin, Jamillah Amer [Faculty of Biosciences and Medical Engineering, Universiti Teknologi Malaysia, Johor Bahru 81310 (Malaysia); Prajitno, Djoko Hadi [Nuclear Technology Center for Materials and Radiometry, National Nuclear Energy, Bandung 40132 (Indonesia); Saidin, Syafiqah [Faculty of Biosciences and Medical Engineering, Universiti Teknologi Malaysia, Johor Bahru 81310 (Malaysia); Nur, Hadi, E-mail: hadi@kimia.fs.utm.my [Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, Johor Bahru 81310 (Malaysia); Department of Physics, Institut Sains dan Teknologi Nasional, Jl. Moh. Kahfi II, Jagakarsa, Jakarta Selatan 12640 (Indonesia); Hermawan, Hendra, E-mail: hendra.hermawan@gmn.ulaval.ca [Department of Mining, Metallurgical and Materials Engineering & CHU de Québec Research Center, Laval University, Québec City G1V 0A6 (Canada)

2015-06-01

Hydroxyapatite (HAp) is an attractive bioceramics due to its similar composition to bone mineral and its ability to promote bone–implant interaction. However, its low strength has limited its application as load bearing implants. This paper presented a work focusing on the improvement of HAp mechanical property by synthesizing iron (Fe)-reinforced bovine HAp nanocomposite powders via mechanosynthesis method. The synthesis process was performed using high energy milling at varied milling time (3, 6, 9, and 12 h). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM). Its mechanical properties were investigated by micro-Vicker's hardness and compression tests. Results showed that milling time directly influenced the characteristics of the nanocomposite powders. Amorphous BHAp was formed after 9 and 12 h milling in the presence of HPO{sub 4}{sup 2−} ions. Continuous milling has improved the crystallinity of Fe without changing the HAp lattice structure. The nanocomposite powders were found in spherical shape, agglomerated and dense after longer milling time. The hardness and Young's modulus of the nanocomposites were also increased at 69% and 66%, respectively, as the milling time was prolonged from 3 to 12 h. Therefore, the improvement of the mechanical properties of nanocomposite was attributed to high Fe crystallinity and homogenous, dense structure produced by mechanosynthesis - Highlights: • Improvement of mechanical properties of HAp bioceramics by mechanosynthesis method • Structure–property relationship of iron–hydroxyapatite ceramic matrix nanocomposite • Milling time influenced the properties of iron–hydroxyapatite ceramic matrix nanocomposite.

Structure–property relationships of iron–hydroxyapatite ceramic matrix nanocomposite fabricated using mechanosynthesis method

International Nuclear Information System (INIS)

Nordin, Jamillah Amer; Prajitno, Djoko Hadi; Saidin, Syafiqah; Nur, Hadi; Hermawan, Hendra

2015-01-01

Hydroxyapatite (HAp) is an attractive bioceramics due to its similar composition to bone mineral and its ability to promote bone–implant interaction. However, its low strength has limited its application as load bearing implants. This paper presented a work focusing on the improvement of HAp mechanical property by synthesizing iron (Fe)-reinforced bovine HAp nanocomposite powders via mechanosynthesis method. The synthesis process was performed using high energy milling at varied milling time (3, 6, 9, and 12 h). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM). Its mechanical properties were investigated by micro-Vicker's hardness and compression tests. Results showed that milling time directly influenced the characteristics of the nanocomposite powders. Amorphous BHAp was formed after 9 and 12 h milling in the presence of HPO 4 2− ions. Continuous milling has improved the crystallinity of Fe without changing the HAp lattice structure. The nanocomposite powders were found in spherical shape, agglomerated and dense after longer milling time. The hardness and Young's modulus of the nanocomposites were also increased at 69% and 66%, respectively, as the milling time was prolonged from 3 to 12 h. Therefore, the improvement of the mechanical properties of nanocomposite was attributed to high Fe crystallinity and homogenous, dense structure produced by mechanosynthesis - Highlights: • Improvement of mechanical properties of HAp bioceramics by mechanosynthesis method • Structure–property relationship of iron–hydroxyapatite ceramic matrix nanocomposite • Milling time influenced the properties of iron–hydroxyapatite ceramic matrix nanocomposite

Surface modification of hydroxyapatite nanoparticles by poly(L-phenylalanine) via ROP of L-phenylalanine N-carboxyanhydride (Pha-NCA)

International Nuclear Information System (INIS)

Dai Yanfeng; Xu Min; Wei Junchao; Zhang Haobin; Chen Yiwang

2012-01-01

The surface of hydroxyapatite nanoparticles was modified by poly(L-phenylalanine) via the ring opening polymerization (ROP) of L-phenylalanine N-carboxyanhydride. The preparation procedure was monitored by Fourier transform infrared spectroscopy (FTIR), and the modified hydroxyapatite was characterized by thermal gravimetric analysis (TGA) and X-ray diffraction (XRD). The results showed that the surface grafting amounts of poly(L-phenylalanine) on HA ranging from 20.26% to 38.92% can be achieved by tuning the reaction condition. The XRD patterns demonstrated that the crystalline structure of the modified hydroxyapatite was nearly the same with that of HA, implying that the ROP was an efficient surface modification method. The MTT assay proved that the biocompatibility of modified HA was very good, which showed the potential application of modified HA in bone tissue engineering.

Synthesis and characterization of hydroxyapatite (HAp) for binder tungstate in 188W/188Re generator system

International Nuclear Information System (INIS)

Eni Hartati; Yati B Yuliyati; Duyeh Setiawan

2014-01-01

In this study, the synthesis of hydroxyapatite has been carried out through a process of precipitation of calcium hydroxide (Ca(OH) 2 ) with phosphoric acid (H 3 PO 4 ) based on acid base reaction process that produce crystalline solid and then it will be used for binder tungstate in 188 W/ 188 Re generator system. The purpose of this study were to characterize the results of synthesized hydroxyapatite and to determine the optimum conditions on generator 188 W/ 188 Re performance such as activation of the heating hydroxyapatite, pH of Na 2 WO 4 , reaction temperature, distribution coefficient and the adsorption capacity (adsorption coefficient) of hydroxyapatite. The characterization of synthesized hydroxyapatite was done using FTIR, XRD and SEM-EDAX, while the determination of the optimum condition of each parameters based on distribution coefficient and adsorption capacity hydroxyapatite using spectrophotometric method. The FTIR results of hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 ) showed the appearance of peaks in the O-H stretching wave number (υ) and 3434.9 cm -1 and 563.8 cm -1 , while the group PO 4 -3 is shown by the P-O bond in (υ) 1033.8 cm -1 . The XRD results indicate that hydroxyapatite had three peaks at 2θ region is 31,875° , 32,205° and 33,080°. Characterization by SEM showed columnar morphology with a particle size of 200 nm. The optimum conditions of each parameter obtained at hydroxyapatite heating temperature 100 °C, Na 2 WO 4 solution pH 3, and the reaction temperature of 60 °C, which gave result on distribution coefficients of 193.74 mL/g and adsorption capacity (adsorption coefficient) of 5.20 mg W/g HAp. (author)

Preparation of hydroxyapatite/zirconia bioceramic nanocomposites for orthopaedic and dental prosthesis applications

Energy Technology Data Exchange (ETDEWEB)

Sung, Yun-Mo [Department of Materials Science and Engineering, Korea University, Seoul 136-713 (Korea, Republic of); Shin, Young-Keun [Technical Support Division, Korloy Incorporated, Cheongjoo-si, Choongbook 361-290 (Korea, Republic of); Ryu, Jae-Jun [Department of Prosthodontics, Medical School, Korea University, Seoul 136-701 (Korea, Republic of)

2007-02-14

Homogeneous mixtures of hydroxyapatite (HAp) and yttria-stabilized zirconia (YSZ) nanoparticles were successfully synthesized using chemical co-precipitation and subsequent calcination. For the synthesis of HAp/YSZ nanopowder, the Ca/P atomic ratio was 1.73 to obtain high-content stoichiometric hydroxyapatite phase and to suppress {beta}-tricalcium phosphate ({beta}-TCP) formation. The agglomerated crystalline powders were milled using YSZ ball media to obtain well-separated nanoparticles. The final particle size of the HAp and YSZ was {approx}50-70 and {approx}15-30 nm, respectively. The crystallinity and morphological feature of the nanopowder was analysed using x-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) analyses. The ball-milled nanopowder mixture was hot pressed at 1100 deg. C for 1 h under 20 MPa in vacuum atmosphere. The sintered HAp/YSZ nanocomposites exhibited approximately 99% of the theoretical density, due not only to the fine nanoscale of the particles, but also to the homogeneous distribution of the nanoparticle mixture. They also showed fine grain structures of the HAp phase due to the suppressed grain growth by YSZ particles. The nanocomposites showed improved mechanical properties, flexural strength of {approx}155 MPa and fracture toughness of {approx}2.1 MP m{sup 1/2}, due to the YSZ contribution to the HAp matrix.

Development and characterization of nanoparticulate formulation of a water soluble prodrug of dexamethasone by HIP complexation.

Science.gov (United States)

Gaudana, Ripal; Parenky, Ashwin; Vaishya, Ravi; Samanta, Swapan K; Mitra, Ashim K

2011-01-01

The objective of this study was to develop and characterize a nanoparticulate-based sustained release formulation of a water soluble dipeptide prodrug of dexamethasone, valine-valine-dexamethasone (VVD). Being hydrophilic in nature, it readily leaches out in the external aqueous medium and hence partitions poorly into the polymeric matrix resulting in minimal entrapment in nanoparticles. Hence, hydrophobic ion pairing (HIP) complexation of the prodrug was employed with dextran sulphate as a complexing polymer. A novel, solid in oil in water emulsion method was employed to encapsulate the prodrug in HIP complex form in poly(lactic-co-glycolic acid) matrix. Nanoparticles were characterized with respect to size, zeta potential, crystallinity of entrapped drug and surface morphology. A significant enhancement in the entrapment of the prodrug in nanoparticles was achieved. Finally, a simple yet novel method was developed which can also be applicable to encapsulate other charged hydrophilic molecules, such as peptides and proteins.

Paramagnetic iron-doped hydroxyapatite nanoparticles with improved metal sorption properties. A bioorganic substrates-mediated synthesis.

Science.gov (United States)

Mercado, D Fabio; Magnacca, Giuliana; Malandrino, Mery; Rubert, Aldo; Montoneri, Enzo; Celi, Luisella; Bianco Prevot, Alessandra; Gonzalez, Mónica C

2014-03-26

This paper describes the synthesis of paramegnetic iron-containing hydroxyapatite nanoparticles and their increased Cu(2+) sorbent capacity when using Ca(2+) complexes of soluble bioorganic substrates from urban wastes as synthesis precursors. A thorough characterization of the particles by TEM, XRD, FTIR spectroscopy, specific surface area, TGA, XPS, and DLS indicates that loss of crystallinity, a higher specific area, an increased surface oxygen content, and formation of surface iron phases strongly enhance Cu(2+) adsorption capacity of hydroxyapatite-based materials. However, the major effect of the surface and morphologycal modifications is the size diminution of the aggregates formed in aqueous solutions leading to an increased effective surface available for Cu(2+) adsorption. Maximum sorption values of 550-850 mg Cu(2+) per gram of particles suspended in an aqueous solution at pH 7 were determined, almost 10 times the maximum values observed for hydroxyapatite nanoparticles suspensions under the same conditions.

Characterization and formation of hydroxyapatite on Ti6Al4V coated by plasma electrolytic oxidation

International Nuclear Information System (INIS)

Durdu, Salih; Deniz, Ömer Faruk; Kutbay, Işıl; Usta, Metin

2013-01-01

Highlights: ► Ti6Al4V alloys were coated by PEO in calcium acetate and β-calcium glycerophosphate. ► Hydroxyapatite and calcium apatite based phases were directly formed on Ti6Al4V. ► Hydroxyapatite coatings were characterized systematically for different times. ► After 5 min, hydroxyapatite and calcium based phases begin to form on the coating. ► HAp on the coating is amorphous due to the rapid solidification during PEO. - Abstract: In this study, Ti6Al4V alloy was coated in the solution consisting of calcium acetate (CA) and β-calcium glycerophosphate (β-Ca-GP) by plasma electrolytic oxidation (PEO) to produce hydroxyapatite and calcium apatite-based composite used as of bioactive and biocompatible materials in biomedical applications. The phase structures, surface morphologies, functional groups of molecules, chemical compositions of the surfaces and the binding energies of atoms in the coating were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and X-ray photoelectron spectroscopy (XPS), respectively. Anatase, rutile, calcium oxide, titanium phosphide, whitlockite, tri-calcium phosphate (TCP), perovskite calcium titanate and hydroxyapatite phases on the coating were detected by XRD analysis. The surface of coatings produced by PEO method has a porous structure. The amount of amorphous hydroxyapatite is the highest value for the coating produced at 5 min in XPS and ATR-FTIR results, whereas the amount of crystalline hydroxyapatite has the highest value for coating produced at 120 min in XRD results.

Ab initio elastic properties and tensile strength of crystalline hydroxyapatite.

Science.gov (United States)

Ching, W Y; Rulis, Paul; Misra, A

2009-10-01

We report elastic constant calculation and a "theoretical" tensile experiment on stoichiometric hydroxyapatite (HAP) crystal using an ab initio technique. These results compare favorably with a variety of measured data. Theoretical tensile experiments are performed on the orthorhombic cell of HAP for both uniaxial and biaxial loading. The results show considerable anisotropy in the stress-strain behavior. It is shown that the failure behavior of the perfect HAP crystal is brittle for tension along the z-axis with a maximum stress of 9.6 GPa at 10% strain. Biaxial failure envelopes from six "theoretical" loading tests show a highly anisotropic pattern. Structural analysis of the crystal under various stages of tensile strain reveals that the deformation behavior manifests itself mainly in the rotation of the PO(4) tetrahedron with concomitant movements of both the columnar and axial Ca ions. These results are discussed in the context of mechanical properties of bioceramic composites relevant to mineralized tissues.

Effect of the deposition temperature on corrosion resistance and biocompatibility of the hydroxyapatite coatings

Energy Technology Data Exchange (ETDEWEB)

Vladescu, A., E-mail: alinava@inoe.ro [National Institute for Optoelectronics, 409 Atomistilor Str., Magurele (Romania); Braic, M. [National Institute for Optoelectronics, 409 Atomistilor Str., Magurele (Romania); Azem, F. Ak [Dokuz Eylul University, Engineering Faculty, Metallurgical and Materials Engineering Department, Buca-Izmir (Turkey); Titorencu, I. [Institute of Cellular Biology and Pathology Nicolae Simionescu of the Romanian Academy, 8 B.P.Hasdeu, Bucharest (Romania); Braic, V. [National Institute for Optoelectronics, 409 Atomistilor Str., Magurele (Romania); Pruna, V. [Institute of Cellular Biology and Pathology Nicolae Simionescu of the Romanian Academy, 8 B.P.Hasdeu, Bucharest (Romania); Kiss, A. [National Institute for Optoelectronics, 409 Atomistilor Str., Magurele (Romania); Parau, A.C.; Birlik, I. [Dokuz Eylul University, Engineering Faculty, Metallurgical and Materials Engineering Department, Buca-Izmir (Turkey)

2015-11-01

Highlights: • Hydroxyapatite has been produced at temperature from 400 to 800 °C by magnetron sputtering. • Hydroxyapatite crystallinity is improved by increasing substrate temperature. • The increase of substrate temperature resulted in corrosion resistance increasing. • The coating shows high growth of the osteosarcoma cells over a wide temperature range. - Abstract: Hydroxyapatite (HAP) ceramics belong to a class of calcium phosphate-based materials, which have been widely used as coatings on titanium medical implants in order to improve bone fixation and thus to increase the lifetime of the implant. In this study, HAP coatings were deposited from pure HAP targets on Ti6Al4V substrates using the radio-frequency magnetron sputtering technique at substrate temperatures ranging from 400 to 800 °C. The surface morphology and the crystallographic structure of the films were investigated by atomic force microscopy (AFM), scanning electron microscopy (SEM) and X-ray diffraction (XRD). The corrosion resistance of the coatings in saliva solution at 37 °C was evaluated by potentiodynamic polarization. Additionally, the human osteosarcoma cell line (MG-63) was used to test the biocompatibility of the coatings. The results showed that all of the coatings grown uniformly and that the increasing substrate temperature induced an increase in their crystallinity. Corrosion performance of the coatings was improved with the increase of the substrate temperature from 400 °C to 800 °C. Furthermore, all the coatings support the attachment and growth of the osteosarcoma cells with regard to the in vitro test findings.

The infrared spectroscopy in the study of the bone crystallinity thermally affected

International Nuclear Information System (INIS)

Medina, C.; Tiesler, V.; Azamar, J.A.; Alvarado G, J.J.; Quintana, P.

2006-01-01

Bone is made up by both organic and inorganic components. Among the latter stands out hydroxyapatite (HAP), composed by hexagonal crystallites arranged in a laminar form. The size of the hydroxyapatite crystals may be altered by different conditions, among those figures thermal exhibition, since during burning the bone eliminates organic matrix and thus promotes the crystallization process of the material. An experimental series was designed to measure crystallinity, in which pig bone remains were burnt at different temperatures and analyzed by infrared spectroscopy (FTIR). By means of analogy a comparison was made between the infrared spectra in order to compare with the ones obtained from the archaeological samples, coming from the Classic period Maya sites of Calakmul and Becan, Campeche. (Author)

Effect of Amino Acids on Morphology of Hydrothermally Synthesized Hydroxyapatite Fibers

Directory of Open Access Journals (Sweden)

QI Mei-li

2017-05-01

Full Text Available Based on the basic principle of biomineralization, hydroxyapatite fiber (HAF with high crystallinity was fabricated via a hydrothermal route with Ca(NO32·4H2O and (NH42HPO4 as the resources, respectively. Effects of the addition of acidic amino acid L-glutamic acid (Glu, neutral amino acid L-phenylalanine (Phe and basic amino acid L-lysine (Lys on the phase composition and morphology of the obtained products were laid special emphasis on. The results show that the products obtained by using the three amino acids are all hydroxyapatite (HA phase with minor CaCO3 in some samples. Meanwhile, all of the amino acids inhibit the growth of the fibers. Spherical morphology exists when Glu is added, the homogeneity of the fibers deteriorates with the addition of Lys. However, rod-like fibers with good uniformity can be obtained with the addition of Phe.

A Comparison of Fatigue Crack Growth in Human Enamel and Hydroxyapatite

OpenAIRE

Bajaj, Devendra; Nazari, Ahmad; Eidelman, Naomi; Arola, Dwayne

2008-01-01

Cracks and craze lines are often observed in the enamel of human teeth, but they rarely cause tooth fracture. The present study evaluates fatigue crack growth in human enamel, and compares that to the fatigue response of sintered hydroxyapatite (HAp) with similar crystallinity, chemistry and density. Miniature inset compact tension (CT) specimens were prepared that embodied a small piece of enamel (N=8) or HAp (N=6). The specimens were subjected to mode I cyclic loads and the steady state cra...

Hydroxyapatite coatings of fracture fixation plates for orthopedic applications

International Nuclear Information System (INIS)

Omar, M.A.; Abdullah, N.S.; Yahya, N.M.; Subuki, I.; Hassan, N.; Mohamad, S.M.

2007-01-01

The plasma sprayed hydroxyapatite (HA) coatings are used on metallic implants to improve their adhesion to bone. The present study investigates the plasma sprayed process of HA on the fracture fixation plates fabricated by metal injection moulding process. The phase and microstructure of the coatings were studied and their microhardness measured. The phase composition of coatings was analyzed by the use of X-ray diffraction method. The homogeneity of the deposit and coating thickness were evaluated using scanning electron microscope (SEM). The results suggest that the nature of the coating morphology, phase and crystallinity changes with respect to the plasma sprayed processing parameters. The XRD revealed the presence of both amorphous and crystalline phases. In addition, the powder particles also melt partially in some region and coating microstructure varied from a porous structure to a smooth glassy structure or a typical lamellar structure. (author)

Thin Bioactive Zn Substituted Hydroxyapatite Coating Deposited on Ultrafine Grained Titanium Substrate: Structure Analysis

Science.gov (United States)

Prosolov, Konstantin A.; Belyavskaya, Olga A.; Muehle, Uwe; Sharkeev, Yurii P.

2018-02-01

Nanocrystalline Zn substituted hydroxyapatite coatings were deposited by radiofrequency magnetron sputtering on the surface of ultrafine-grained titanium substrates. Cross section transmission electron microscopy provided information about the morphology and texture of the thin film while in-column energy dispersive X-ray analysis confirmed the presence of Zn in the coating. The Zn substituted hydroxyapatite coating was formed by an equiaxed polycrystalline grain structure. Effect of substrate crystallinity on the structure of deposited coating is discussed. An amorphous TiO2 sublayer of 8 nm thickness was detected in the interface between the polycrystalline coating and the Ti substrate. Its appearance in the amorphous state is attributed to prior to deposition etching of the substrate and subsequent condensation of oxygen-containing species sputtered from the target. This layer contributes to the high coating-to-substrate adhesion. The major P-O vibrational modes of high intensity were detected by Raman spectroscopy. The Zn substituted hydroxyapatite could be a material of choice when antibacterial osteoconductive coating with a possibility of withstanding mechanical stress during implantation and service is needed.

Thin Bioactive Zn Substituted Hydroxyapatite Coating Deposited on Ultrafine-Grained Titanium Substrate: Structure Analysis

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Konstantin A. Prosolov

2018-02-01

Full Text Available Nanocrystalline Zn-substituted hydroxyapatite coatings were deposited by radiofrequency magnetron sputtering on the surface of ultrafine-grained titanium substrates. Cross-section transmission electron microscopy provided information about the morphology and texture of the thin film while in-column energy dispersive X-ray analysis confirmed the presence of Zn in the coating. The Zn-substituted hydroxyapatite coating was formed by an equiaxed polycrystalline grain structure. Effect of substrate crystallinity on the structure of deposited coating is discussed. An amorphous TiO2 sublayer of 8-nm thickness was detected in the interface between the polycrystalline coating and the Ti substrate. Its appearance in the amorphous state is attributed to prior to deposition etching of the substrate and subsequent condensation of oxygen-containing species sputtered from the target. This layer contributes to the high coating-to-substrate adhesion. The major P–O vibrational modes of high intensity were detected by Raman spectroscopy. The Zn-substituted hydroxyapatite could be a material of choice when antibacterial osteoconductive coating with a possibility of withstanding mechanical stress during implantation and service is needed.

Photocatalytic degradation of paraoxon-ethyl in aqueous solution using titania nanoparticulate film

International Nuclear Information System (INIS)

Prasad, G.K.; Ramacharyulu, P.V.R.K.; Kumar, J. Praveen; Srivastava, A.R.; Singh, Beer

2012-01-01

Photocatalytic degradation of paraoxon-ethyl (o,o-diethyl o-(4-nitrophenyl) phosphate), a well known surrogate of chemical warfare agents, in aqueous solution was studied by using titania nanoparticulate film. Reaction followed pseudo first order behaviour. Photolytic degradation reaction of paraoxon-ethyl demonstrated relatively low rate with a value of rate constant of 2.5 × 10 −3 min −1 . Whereas, degradation reaction in the presence of titania nanoparticulate film and UV light displayed enhanced rate with a value of rate constant of 6.9 × 10 −3 min −1 due to photocatalysis. Gas chromatography–mass spectrometry analysis showed the formation of p-nitrophenol, o,o-diethyl phosphonic acid, o-ethyl, diphosphonic acid, phosphoric acid, dimerized product of o,o-diethyl phosphonic acid, acetaldehyde, and carbon dioxide due to photocatalytic degradation of paraoxon-ethyl. It indicates that, photocatalytic degradation reaction begins with destruction of P–O–C bonds. Subsequently, P, C atoms were found to be oxidized gradually, and contributed to its photocatalytic degradation. - Highlights: ► Synthesis of titania nanoparticles by sol–gel method. ► Fabrication of titania nanoparticulate film by dip coating. ► Paraoxon ethyl degradation reactions followed pseudo first order behaviour. ► Paraoxon-ethyl degraded to non toxic compounds like CO 2 , acetaldehyde, and nitrophenol.

Synthesis and morphology of hydroxyapatite/polyethylene oxide nanocomposites with block copolymer compatibilized interfaces

Science.gov (United States)

Lee, Ji Hoon; Shofner, Meisha

2012-02-01

In order to exploit the promise of polymer nanocomposites, special consideration should be given to component interfaces during synthesis and processing. Previous results from this group have shown that nanoparticles clustered into larger structures consistent with their native shape when the polymer matrix crystallinity was high. Therefore in this research, the nanoparticles are disguised from a highly-crystalline polymer matrix by cloaking them with a matrix-compatible block copolymer. Specifically, spherical and needle-shaped hydroxyapatite nanoparticles were synthesized using a block copolymer templating method. The block copolymer used, polyethylene oxide-b-polymethacrylic acid, remained on the nanoparticle surface following synthesis with the polyethylene oxide block exposed. These nanoparticles were subsequently added to a polyethylene oxide matrix using solution processing. Characterization of the nanocomposites indicated that the copolymer coating prevented the nanoparticles from assembling into ordered clusters and that the matrix crystallinity was decreased at a nanoparticle spacing of approximately 100 nm.

Labilities of aqueous nanoparticulate metal complexes in environmental speciation analysis

NARCIS (Netherlands)

Town, R.M.; Leeuwen, van H.P.

2014-01-01

An inherent property of a dispersion of charged nanoparticles is that their charges and reactive sites are spatially confined to the particle body which is at a different potential from that in the bulk medium. This feature has important consequences for the reactivity of nanoparticulate

Effect of modification substrate on the microstructure of hydroxyapatite coating

International Nuclear Information System (INIS)

Realpe-Jaramillo, J; Morales-Morales, J A; González-Sánchez, J A; Cabanzo, R; Mejía-Ospino, E; Rodríguez-Pereira, J

2017-01-01

Bioactive hydroxyapatite (HA) coatings were fabricated by a precipitation, sol-gel and dip-coating method. The effects of the aging time and the base used to adjust pH and substrate materials on the phases and microstructures of HA coatings were studied by field emission scanning electron microscopy FESEM, energy dispersive spectroscopy EDS, X-ray photoelectron spectroscopy XPS, and the vibrations of the phosphate groups were determined by Raman spectroscopy. The results showed that all the films were composed of the phases of TiO 2 and HA. With coated titanium substrate with TiO 2 , the crystallinity of the HA coating increases, the structure became more compact and the Ca/P ratio increased because of the loss of P in the films. The addition of sodium hydroxide (adjusting the pH level to about 10) can increase the HA content in the coating. XPS and EDS results for steel substrate and titanium showed poor calcium content as obtained with a Ca/P ratio of 1.38 and 1.58, respectively, composition is similar to that of natural apatite. However, spectroscopic results suggest the presence of a mixture of hydroxyapatite and octacalcium phosphate. The different substrate materials have a high influence on the microstructure of the separated double films. However, hydroxyapatite nanopowders coatings were obtained using a simple method, with potential biomedical applications. (paper)

Effect of modification substrate on the microstructure of hydroxyapatite coating

Science.gov (United States)

Realpe-Jaramillo, J.; Morales-Morales, J. A.; González-Sánchez, J. A.; Cabanzo, R.; Mejía-Ospino, E.; Rodríguez-Pereira, J.

2017-01-01

Bioactive hydroxyapatite (HA) coatings were fabricated by a precipitation, sol-gel and dip-coating method. The effects of the aging time and the base used to adjust pH and substrate materials on the phases and microstructures of HA coatings were studied by field emission scanning electron microscopy FESEM, energy dispersive spectroscopy EDS, X-ray photoelectron spectroscopy XPS, and the vibrations of the phosphate groups were determined by Raman spectroscopy. The results showed that all the films were composed of the phases of TiO2 and HA. With coated titanium substrate with TiO2, the crystallinity of the HA coating increases, the structure became more compact and the Ca/P ratio increased because of the loss of P in the films. The addition of sodium hydroxide (adjusting the pH level to about 10) can increase the HA content in the coating. XPS and EDS results for steel substrate and titanium showed poor calcium content as obtained with a Ca/P ratio of 1.38 and 1.58, respectively, composition is similar to that of natural apatite. However, spectroscopic results suggest the presence of a mixture of hydroxyapatite and octacalcium phosphate. The different substrate materials have a high influence on the microstructure of the separated double films. However, hydroxyapatite nanopowders coatings were obtained using a simple method, with potential biomedical applications.

Synthesis, Structure, and Luminescent Properties of Europium-Doped Hydroxyapatite Nanocrystalline Powders

Directory of Open Access Journals (Sweden)

Carmen Steluta Ciobanu

2012-01-01

Full Text Available The luminescent europium-doped hydroxyapatite (Eu:HAp, Ca10−xEux(PO46(OH2 with 0≤x≤0.2 nanocrystalline powders was synthesized by coprecipitation. The structural, morphological, and textural properties were well characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The vibrational studies were performed by Fourier transform infrared, Raman, and photoluminescence spectroscopies. The X-ray diffraction analysis revealed that hydroxyapatite is the unique crystalline constituent of all the samples, indicating that Eu has been successfully inserted into the HAp lattice. Eu doping inhibits HAp crystallization, leading to a decrease of the average crystallite size from around 20 nm in the undoped sample to around 7 nm in the sample with the highest Eu concentration. Furthermore, the samples show the characteristic 5D0→7F0 transition observed at 578 nm related to Eu3+ ions distributed on Ca2+ sites of the apatitic structure.

Synthesis, Structure, and Luminescent Properties of Europium-Doped Hydroxyapatite Nanocrystalline Powders

International Nuclear Information System (INIS)

Ciobanu, C.S.; Iconaru, S.L.; Predoi, D.; Massuyeau, F.; Constantin, L.V.; Costescu, A.

2012-01-01

The luminescent europium-doped hydroxyapatite (Eu:HAp, Ca 10-x Eu x (PO 4 ) 6 (OH) 2 ) with 0>x>0.2 nanocrystalline powders was synthesized by coprecipitation. The structural, morphological, and textural properties were well characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The vibrational studies were performed by Fourier transform infrared, Raman, and photoluminescence spectroscopies. The X-ray diffraction analysis revealed that hydroxyapatite is the unique crystalline constituent of all the samples, indicating that Eu has been successfully inserted into the HAp lattice. Eu doping inhibits HAp crystallization, leading to a decrease of the average crystallite size from around 20 nm in the undoped sample to around 7 nm in the sample with the highest Eu concentration. Furthermore, the samples show the characteristic 5 D 0 → 7 F 0 transition observed at 578 nm related to Eu 3+ ions distributed on Ca 2+ sites of the apatitic structure

Deposition of crystalline hydroxyapatite nano-particle on zirconia ceramic: a potential solution for the poor bonding characteristic of zirconia ceramics to resin cement.

Science.gov (United States)

Azari, Abbas; Nikzad, Sakineh; Yazdani, Arash; Atri, Faezeh; Fazel Anvari-Yazdi, Abbas

2017-07-01

The poor bonding strength of zirconia to different dental substrates is one of the challenging issues in restorative dentistry. Hydroxyapatite is an excellent biocompatible material with fine bonding properties. In this study, it was hypothesized that hydroxyapatite coating on zirconia would improve its bond strength. Forty-five zirconia blocks were prepared and randomly divided into three groups: hydroxyapatite coating, sandblasting, and no preparation (control). The blocks were bonded to cement and the micro-shear bond strength was measured following load application. The bond strength values were analyzed with the Kruskal-Wallis test in 3 groups and paired comparisons were made using the Mann-Whitney U test. The failure patterns of the specimens were studied by a stereomicroscope and a scanning electron microscope and then analyzed by the chi-square test (significance level = 0.05). Deposition of hydroxyapatite on the zirconia surface significantly improved its bond strength to the resin cement in comparison with the control specimens (p improved the bond strength quality and values.

XANES analysis of calcium and sodium phosphates and silicates and hydroxyapatite-Bioglass (registered) 45S5 co-sintered bioceramics

International Nuclear Information System (INIS)

Demirkiran, Hande; Hu Yongfeng; Zuin, Lucia; Appathurai, Narayana; Aswath, Pranesh B.

2011-01-01

Bioglass (registered) 45S5 was co-sintered with hydroxyapatite at 1200 deg. C. When small amounts ( 5 (PO 4 ) 2 SiO 4 and Na 3 Ca 6 (PO 4 ) 5 in an amorphous silicate matrix respectively. These chemistries show improved bioactivity compared to hydroxyapatite and are the subject of this study. The structure of several crystalline calcium and sodium phosphates and silicates as well as the co-sintered hydroxyapatite-Bioglass (registered) 45S5 bioceramics were examined using XANES spectroscopy. The nature of the crystalline and amorphous phases were studied using silicon (Si) and phosphorus (P) K- and L 2,3 -edge and calcium (Ca) K-edge XANES. Si L 2,3 -edge spectra of sintered bioceramic compositions indicates that the primary silicates present in these compositions are sodium silicates in the amorphous state. From Si K-edge spectra, it is shown that the silicates are in a similar structural environment in all the sintered bioceramic compositions with 4-fold coordination. Using P L 2,3 -edge it is clearly shown that there is no evidence of sodium phosphate present in the sintered bioceramic compositions. In the P K-edge spectra, the post-edge shoulder peak at around 2155 eV indicates that this shoulder to be more defined for calcium phosphate compounds with decreasing solubility and increasing thermodynamic stability. This shoulder peak is more noticeable in hydroxyapatite and β-TCP indicating greater stability of the phosphate phase. The only spectra that does not show a noticeable peak is the composition with Na 3 Ca 6 (PO 4 ) 5 in a silicate matrix indicating that it is more soluble compared to the other compositions.

Three-phase bone scintigraphy of hydroxyapatite ocular implants

International Nuclear Information System (INIS)

Leitha, T.; Staudenherz, A.; Scholz, U.

1995-01-01

Hydroxyapatite ocular implants are replicas of lamellar bone tissue derived from the exoskeleton of a reef-building coral by a hydrothermal chemical exchange reaction. Attached to the eye muscles, they act as a passive framework for fibrovascular ingrowth and can be drilled to hold the visible part of the artificial eye and allow synchronous eye movement. Fibrovascular ingrowth has to be confirmed by bone scintigraphy before the drilling procedure. This study monitored the vascular ingrowth into the implant in ten patients over 12 months to establish a clinically feasible imaging protocol. Tracer accumulation was monitored visually and quantitatively in dynamic and single-photon emission tomography (SPET) scans after the intravenous administration of 600 MBq of 99m Tc-DPD. The implants showed no tracer accumulation in the arterial or blood pool phase. Accordingly, dynamic scintigraphy can be omitted from the imaging protocol. Delayed tracer accumulation appeared no earlier than 2 and no later than 6 months after surgery. Planar scintigraphy is not recommended as high-resolution SPET is necessary to separate the implant from the surrounding bone. We conclude that imaging can be confined to high-resolution SPET 3 h after tracer injection, no earlier than 3 months after surgery. The vascularized hydroxyapatite orbital implant is an important in vivo model for bone-seeking agents to study their uptake kinetics independently of any soft tissue and bone disease. Our results provide evidence that in normal bones the chemical adsorption of 99m Tc-DPD into the crystalline structure of hydroxyapatite is the only quantitatively relevant uptake mechanism. (orig.)

Three-phase bone scintigraphy of hydroxyapatite ocular implants

Energy Technology Data Exchange (ETDEWEB)

Leitha, T. [Univ. Clinic of Nuclear Medicine, Univ. of Vienna (Austria); Staudenherz, A. [Univ. Clinic of Nuclear Medicine, Univ. of Vienna (Austria); Scholz, U. [First Univ. Clinic of Ophthalmology, Univ. of Vienna (Austria)

1995-04-01

Hydroxyapatite ocular implants are replicas of lamellar bone tissue derived from the exoskeleton of a reef-building coral by a hydrothermal chemical exchange reaction. Attached to the eye muscles, they act as a passive framework for fibrovascular ingrowth and can be drilled to hold the visible part of the artificial eye and allow synchronous eye movement. Fibrovascular ingrowth has to be confirmed by bone scintigraphy before the drilling procedure. This study monitored the vascular ingrowth into the implant in ten patients over 12 months to establish a clinically feasible imaging protocol. Tracer accumulation was monitored visually and quantitatively in dynamic and single-photon emission tomography (SPET) scans after the intravenous administration of 600 MBq of {sup 99m}Tc-DPD. The implants showed no tracer accumulation in the arterial or blood pool phase. Accordingly, dynamic scintigraphy can be omitted from the imaging protocol. Delayed tracer accumulation appeared no earlier than 2 and no later than 6 months after surgery. Planar scintigraphy is not recommended as high-resolution SPET is necessary to separate the implant from the surrounding bone. We conclude that imaging can be confined to high-resolution SPET 3 h after tracer injection, no earlier than 3 months after surgery. The vascularized hydroxyapatite orbital implant is an important in vivo model for bone-seeking agents to study their uptake kinetics independently of any soft tissue and bone disease. Our results provide evidence that in normal bones the chemical adsorption of {sup 99m}Tc-DPD into the crystalline structure of hydroxyapatite is the only quantitatively relevant uptake mechanism. (orig.)

Polymer-Assisted Hydrothermal Synthesis of Hierarchically Arranged Hydroxyapatite Nanoceramic

Directory of Open Access Journals (Sweden)

A. Joseph Nathanael

2013-01-01

Full Text Available Flower-like hydroxyapatite (HA nanostructures were synthesized by a polymer-assisted hydrothermal method. The thickness of the petals/plates decreased from 200 nm to 40 nm as the polymer concentration increased. The thickness also decreased as the hydrothermal treatment time increased from 6 to 12 hr. The HRTEM and SAED patterns suggest that the floral-like HA nanostructures are single crystalline in nature. Structural analysis based on XRD and Raman experiments implied that the produced nanostructure is a pure form of HA without any other impurities. The possible formation mechanism was discussed for the formation of flower-like HA nanostructures during polymer-assisted hydrothermal synthesis. Finally, in vitro cellular analysis revealed that the hierarchically arranged HA nanoceramic had improved cell viability relative to other structures. The cells were actively proliferated over these nanostructures due to lower cytotoxicity. Overall, the size and the crystallinity of the nanostructures played a role in improving the cell proliferation.

Hydroxyapatite coatings with oriented nanoplate and nanorod arrays: Fabrication, morphology, cytocompatibility and osteogenic differentiation

Energy Technology Data Exchange (ETDEWEB)

Chen, Wei [The Education Ministry Key Lab of Resource Chemistry and Shanghai Key Laboratory of Rare Earth Functional Materials, Shanghai Normal University, Shanghai 200234 (China); Tian, Bo [Shanghai Key Laboratory of Orthopedic Implant, Department of Orthopedic Surgery, Shanghai Ninth People' s Hospital, Shanghai Jiao Tong University School of Medicine, Shanghai 200011 (China); Lei, Yong; Ke, Qin-Fei [The Education Ministry Key Lab of Resource Chemistry and Shanghai Key Laboratory of Rare Earth Functional Materials, Shanghai Normal University, Shanghai 200234 (China); Zhu, Zhen-An, E-mail: zhuzhenan2006@126.com [Shanghai Key Laboratory of Orthopedic Implant, Department of Orthopedic Surgery, Shanghai Ninth People' s Hospital, Shanghai Jiao Tong University School of Medicine, Shanghai 200011 (China); Guo, Ya-Ping, E-mail: ypguo@shnu.edu.cn [The Education Ministry Key Lab of Resource Chemistry and Shanghai Key Laboratory of Rare Earth Functional Materials, Shanghai Normal University, Shanghai 200234 (China)

2016-10-01

Hydroxyapatite (HA) crystals exhibit rod-like shape with c-axis orientation and plate-like shape with a(b)-axis orientation in vertebrate bones and tooth enamel surfaces, respectively. Herein, we report the synthesis of HA coatings with the oriented nanorod arrays (RHACs) and HA coatings with oriented nanoplate arrays (PHACs) by using bioglass coatings as sacrificial templates. After soaking in simulated body fluid (SBF) at 120 °C, the bioglass coatings are hydrothermally converted into the HA coatings via a dissolution-precipitation reaction. If the Ca/P ratios in SBF are 2.50 and 1.25, the HA crystals on the coatings are oriented nanorod arrays and oriented nanoplate arrays, respectively. Moreover, the bioglass coatings are treated with SBF at 37 °C, plate-like HA coatings with a low crystallinity (SHACs) are prepared. As compared with the Ti6Al4V and SHACs, the human bone marrow stromal cells (hBMSCs) on the RHACs and PHACs have better cell adhesion, spreading, proliferation and osteogenic differentiation because of their moderately hydrophilic surfaces and similar chemical composition, morphology and crystal orientation to human hard tissues. Notably, the morphologies of HA crystals have no obvious effects on cytocompatibility and osteogenic differentiation. Hence, the HA coatings with oriented nanoplate arrays or oriented nanorod arrays have a great potential for orthopedic applications. - Highlights: • We prepare hydroxyapatite coatings with oriented nanoplate and nanorod arrays. • Hydroxyapatite coatings are in situ converted from bioglass coatings. • Hydroxyapatite coatings have good cytocompatibility and osteogenic differentiation. • Oriented hydroxyapatite coatings are used for orthopedic implants.

Hydroxyapatite coatings with oriented nanoplate and nanorod arrays: Fabrication, morphology, cytocompatibility and osteogenic differentiation

International Nuclear Information System (INIS)

Chen, Wei; Tian, Bo; Lei, Yong; Ke, Qin-Fei; Zhu, Zhen-An; Guo, Ya-Ping

2016-01-01

Hydroxyapatite (HA) crystals exhibit rod-like shape with c-axis orientation and plate-like shape with a(b)-axis orientation in vertebrate bones and tooth enamel surfaces, respectively. Herein, we report the synthesis of HA coatings with the oriented nanorod arrays (RHACs) and HA coatings with oriented nanoplate arrays (PHACs) by using bioglass coatings as sacrificial templates. After soaking in simulated body fluid (SBF) at 120 °C, the bioglass coatings are hydrothermally converted into the HA coatings via a dissolution-precipitation reaction. If the Ca/P ratios in SBF are 2.50 and 1.25, the HA crystals on the coatings are oriented nanorod arrays and oriented nanoplate arrays, respectively. Moreover, the bioglass coatings are treated with SBF at 37 °C, plate-like HA coatings with a low crystallinity (SHACs) are prepared. As compared with the Ti6Al4V and SHACs, the human bone marrow stromal cells (hBMSCs) on the RHACs and PHACs have better cell adhesion, spreading, proliferation and osteogenic differentiation because of their moderately hydrophilic surfaces and similar chemical composition, morphology and crystal orientation to human hard tissues. Notably, the morphologies of HA crystals have no obvious effects on cytocompatibility and osteogenic differentiation. Hence, the HA coatings with oriented nanoplate arrays or oriented nanorod arrays have a great potential for orthopedic applications. - Highlights: • We prepare hydroxyapatite coatings with oriented nanoplate and nanorod arrays. • Hydroxyapatite coatings are in situ converted from bioglass coatings. • Hydroxyapatite coatings have good cytocompatibility and osteogenic differentiation. • Oriented hydroxyapatite coatings are used for orthopedic implants.

Biomimetic composite microspheres of collagen/chitosan/nano-hydroxyapatite: In-situ synthesis and characterization.

Science.gov (United States)

Teng, Shu-Hua; Liang, Mian-Hui; Wang, Peng; Luo, Yong

2016-01-01

The collagen/chitosan/hydroxyapatite (COL/CS/HA) composite microspheres with a good spherical form and a high dispersity were successfully obtained using an in-situ synthesis method. The FT-IR and XRD results revealed that the inorganic phase in the microspheres was crystalline HA containing carbonate ions. The morphology of the composite microspheres was dependent on the HA content, and a more desirable morphology was achieved when 20 wt.% HA was contained. The composite microspheres exhibited a narrow particle distribution, most of which ranged from 5 to 10 μm. In addition, the needle-like HA nano-particles were uniformly distributed in the composite microspheres, and their crystallinity and crystal size decreased with the HA content. Copyright © 2015 Elsevier B.V. All rights reserved.

The synthesis of hydroxyapatite with different crystallinities by controlling the concentration of recombinant CEMP1 for biological application

Energy Technology Data Exchange (ETDEWEB)

Chen, Xiaofeng [Hospital of Stomatology, Medical School of Nanjing University, Nanjing, Jiangsu 210093 (China); Liu, Yu, E-mail: lyvette@163.com [Hospital of Stomatology, Medical School of Nanjing University, Nanjing, Jiangsu 210093 (China); Yang, Jie; Wu, Wenlei; Miao, Leiying; Yu, Yijun [Hospital of Stomatology, Medical School of Nanjing University, Nanjing, Jiangsu 210093 (China); Yang, Xuebin [Biomaterials and Tissue Engineering Group, Leeds Dental Institute, University of Leeds (United Kingdom); Sun, Weibin, E-mail: wbsun@nju.edu.cn [Hospital of Stomatology, Medical School of Nanjing University, Nanjing, Jiangsu 210093 (China)

2016-02-01

Cementum protein 1 (CEMP1) has been reported to be cementum specific and it plays a role in the properties and structure of cementum mineralization. This study was carried out to test the hypothesis that, CEMP1 had the capacity to guide ordered HA formation as it accumulated at targeting site. Crystals induced by protein were prepared by biomimetic method. The effects of CEMP1 concentrations (0–100 μg/ml) on the rate of calcium phosphate precipitation was monitored during 48 h, while the formed mineral phases were assessed utilizing transmission electron microscope (TEM), selected area electron diffraction (SAED), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The results showed that recombinant cementum protein 1 (rhCEMP1) affected the crystal nucleation and growth. At lower rhCEMP1 concentrations (0–50 μg/ml), limited mineral formation occurred and only small bundles of HA crystals were found. However, with 100 μg/ml of rhCEMP1, a predominance of organized linear needle-like HA crystals was observed. FTIR revealed the characteristic bands of HA appearing at 1106 cm{sup −1}, 557 cm{sup −1}, and 598 cm{sup −1}. Therefore, increasing the concentration of rhCEMP1 can lead to the formation of ordered bundles of HA crystals in vitro. - Highlights: • We produce recombinant human cementum protein 1 (rhCEMP1). • We synthesize hydroxyapatite/rhCEMP1 with different crystallinities. • Increase of rhCEMP1 leads to the formation of ordered bundles of HA crystals.

Photocatalytic degradation of paraoxon-ethyl in aqueous solution using titania nanoparticulate film

Energy Technology Data Exchange (ETDEWEB)

Prasad, G.K., E-mail: gkprasad2001@yahoo.com; Ramacharyulu, P.V.R.K.; Kumar, J. Praveen; Srivastava, A.R.; Singh, Beer

2012-06-30

Photocatalytic degradation of paraoxon-ethyl (o,o-diethyl o-(4-nitrophenyl) phosphate), a well known surrogate of chemical warfare agents, in aqueous solution was studied by using titania nanoparticulate film. Reaction followed pseudo first order behaviour. Photolytic degradation reaction of paraoxon-ethyl demonstrated relatively low rate with a value of rate constant of 2.5 Multiplication-Sign 10{sup -3} min{sup -1}. Whereas, degradation reaction in the presence of titania nanoparticulate film and UV light displayed enhanced rate with a value of rate constant of 6.9 Multiplication-Sign 10{sup -3} min{sup -1} due to photocatalysis. Gas chromatography-mass spectrometry analysis showed the formation of p-nitrophenol, o,o-diethyl phosphonic acid, o-ethyl, diphosphonic acid, phosphoric acid, dimerized product of o,o-diethyl phosphonic acid, acetaldehyde, and carbon dioxide due to photocatalytic degradation of paraoxon-ethyl. It indicates that, photocatalytic degradation reaction begins with destruction of P-O-C bonds. Subsequently, P, C atoms were found to be oxidized gradually, and contributed to its photocatalytic degradation. - Highlights: Black-Right-Pointing-Pointer Synthesis of titania nanoparticles by sol-gel method. Black-Right-Pointing-Pointer Fabrication of titania nanoparticulate film by dip coating. Black-Right-Pointing-Pointer Paraoxon ethyl degradation reactions followed pseudo first order behaviour. Black-Right-Pointing-Pointer Paraoxon-ethyl degraded to non toxic compounds like CO{sub 2}, acetaldehyde, and nitrophenol.

Direct morphological comparison of vacuum plasma sprayed and detonation gun sprayed hydroxyapatite coatings for orthopaedic applications.

Science.gov (United States)

Gledhill, H C; Turner, I G; Doyle, C

1999-02-01

Hydroxyapatite coatings on titanium substrates were produced using two thermal spray techniques vacuum plasma spraying and detonation gun spraying. X-ray diffraction was used to compare crystallinity and residual stresses in the coatings. Porosity was measured using optical microscopy in conjunction with an image analysis system. Scanning electron microscopy and surface roughness measurements were used to characterise the surface morphologies of the coatings. The vacuum plasma sprayed coatings were found to have a lower residual stress, a higher crystallinity and a higher level of porosity than the detonation gun coatings. It is concluded that consideration needs to be given to the significance of such variations within the clinical context.

Characterization of hydroxyapatite coatings deposited by hydrothermal electrochemical method on NaOH immersed Ti6Al4V

International Nuclear Information System (INIS)

He, Daihua; Liu, Ping; Liu, Xinkuan; Ma, Fengcang; Chen, Xiaohong; Li, Wei; Du, Jiandi; Wang, Pu; Zhao, Jun

2016-01-01

The hydrothermal electrochemical method was used to deposit hydroxyapatite coating on Ti6Al4V. In order to improve the bonding strength between the coating and substrate, the substrates were modified by 8 M NaOH solution before the deposition. The effects of immersing time on the substrate, on the hydroxyapatite coating, and on the bonding strength were studied. X-Ray Diffraction, Scanning Electron Microscope, Fourier Transform Infrared Spectroscopy and Drop Shape Analysis Method were applied. And the crystallinity of hydroxyapatite coating was calculated. The results show that immersing treatment effects the phase compositions, the microstructure and the wettability of the substrate surface. A porous, three-dimensional network structure is formed on the Ti6Al4V surface through the NaOH immersion. The pore size and depth increase with the increase of immersing time from 12 to 48 h. The surface microstructure of Ti6Al4V with 60 h′ immersion time was different from the others. The modification treatment can improve the bonding strength between hydroxyapatite coating and the substrate obviously. The value of the bonding strength with the substrate immersed for 48 h is larger than those of the others. A bone-like apatite layer forms on the coating after 3 days of soaking in SBF, implying with good bioactivity of the hydroxyapatite coatings deposited by the method. The surface characteristics of the sample immersed with 48 h are more conductive to the deposition of hydroxyapatite and to the improvement of the bonding strength. The formation mechanism of hydroxyapatite coating deposited by hydrothermal electrochemical method was discussed. - Highlights: • Immerse Ti6Al4V alloy with NaOH solution for different immersing time. • We deposit hydroxyapatite coating by hydrothermal electrochemical method. • We examine changes of composition, microstructure, bonding strength and bioactivity of the hydroxyapatite coating. • 48 h is the optimal immersing time. • We

XANES analysis of calcium and sodium phosphates and silicates and hydroxyapatite-Bioglass (registered) 45S5 co-sintered bioceramics

Energy Technology Data Exchange (ETDEWEB)

Demirkiran, Hande [Graduate Student, Materials Science and Engineering Department, University of Texas at Arlington, Arlington, TX (United States); Hu Yongfeng; Zuin, Lucia [Beamline Scientist, Canadian Light Source, Saskatoon, SK (Canada); Appathurai, Narayana [Beamline Scientist, Synchrotron Radiation Center, Madison, WI (United States); Aswath, Pranesh B., E-mail: aswath@uta.edu [Materials Science and Engineering Department, University of Texas at Arlington, Arlington, TX (United States)

2011-03-12

Bioglass (registered) 45S5 was co-sintered with hydroxyapatite at 1200 deg. C. When small amounts (< 5 wt.%) of Bioglass (registered) 45S5 was added it behaved as a sintering aid and also enhanced the decomposition of hydroxyapatite to {beta}-tricalcium phosphate. However when 10 wt.% and 25 wt.% Bioglass (registered) 45S5 was used it resulted in the formation of Ca{sub 5}(PO{sub 4}){sub 2}SiO{sub 4} and Na{sub 3}Ca{sub 6}(PO{sub 4}){sub 5} in an amorphous silicate matrix respectively. These chemistries show improved bioactivity compared to hydroxyapatite and are the subject of this study. The structure of several crystalline calcium and sodium phosphates and silicates as well as the co-sintered hydroxyapatite-Bioglass (registered) 45S5 bioceramics were examined using XANES spectroscopy. The nature of the crystalline and amorphous phases were studied using silicon (Si) and phosphorus (P) K- and L{sub 2,3}-edge and calcium (Ca) K-edge XANES. Si L{sub 2,3}-edge spectra of sintered bioceramic compositions indicates that the primary silicates present in these compositions are sodium silicates in the amorphous state. From Si K-edge spectra, it is shown that the silicates are in a similar structural environment in all the sintered bioceramic compositions with 4-fold coordination. Using P L{sub 2,3}-edge it is clearly shown that there is no evidence of sodium phosphate present in the sintered bioceramic compositions. In the P K-edge spectra, the post-edge shoulder peak at around 2155 eV indicates that this shoulder to be more defined for calcium phosphate compounds with decreasing solubility and increasing thermodynamic stability. This shoulder peak is more noticeable in hydroxyapatite and {beta}-TCP indicating greater stability of the phosphate phase. The only spectra that does not show a noticeable peak is the composition with Na{sub 3}Ca{sub 6}(PO{sub 4}){sub 5} in a silicate matrix indicating that it is more soluble compared to the other compositions.

Hydroxyapatite-chitosan based bioactive hybrid biomaterials with improved mechanical strength

Science.gov (United States)

Zima, A.

2018-03-01

Composites consisting of hydroxyapatite (HA) and chitosan (CTS) have recently been intensively studied. In this work, a novel inorganic-organic (I/O) HA/CTS materials in the form of granules were prepared through a simple solution-based chemical method. During the synthesis of these hybrids, the electrostatic complexes between positively charged, protonated amine groups of chitosan and the negative phosphate species (HPO42 - and H2PO4-) were formed. Our biocomposites belong to the class I of hybrids, which was confirmed by FTIR studies. XRD analysis revealed that the obtained materials consisted of hydroxyapatite as the only crystalline phase. Homogeneous dispersion of the components in HA/CTS composites was confirmed. The use of 17 wt% and 23 wt% of chitosan resulted in approximately 12-fold and 16-fold increase in the compressive strength of HA/CTS as compared to the non-modified HA material. During incubation of the studied materials in SBF, pH of the solution remained close to the physiological one. Formation of apatite layer on their surfaces indicated bioactive nature of the developed biomaterials.

Hydroxyapatite-diamondlike carbon nanocomposite films

International Nuclear Information System (INIS)

Narayan, Roger J.

2005-01-01

Hydroxyapatite is a bioactive ceramic that mimics the mineral composition of natural bone. Conventional plasma-sprayed hydroxyapatite coatings demonstrate poor adhesion and poor mechanical integrity. We have developed hydroxyapatite-diamondlike carbon bilayer film. The diamondlike carbon interlayer serves to prevent metal ion release and improve adhesion of the hydroxyapatite film. These films were characterized using X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, nanoindentation, and microscratch adhesion testing. Based on the results of this study, hydroxyapatite-diamondlike carbon bilayers demonstrate promise for use in several orthopedic implants

Hydroxyapatite-diamondlike carbon nanocomposite films

Energy Technology Data Exchange (ETDEWEB)

Narayan, Roger J. [School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, GA 30332-0245 (United States)]. E-mail: roger.narayan@mse.gatech.edu

2005-05-15

Hydroxyapatite is a bioactive ceramic that mimics the mineral composition of natural bone. Conventional plasma-sprayed hydroxyapatite coatings demonstrate poor adhesion and poor mechanical integrity. We have developed hydroxyapatite-diamondlike carbon bilayer film. The diamondlike carbon interlayer serves to prevent metal ion release and improve adhesion of the hydroxyapatite film. These films were characterized using X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, nanoindentation, and microscratch adhesion testing. Based on the results of this study, hydroxyapatite-diamondlike carbon bilayers demonstrate promise for use in several orthopedic implants.

Microwave assisted synthesis of nano sized sulphate doped hydroxyapatite

International Nuclear Information System (INIS)

Alshemary, Ammar Z.; Goh, Yi-Fan; Akram, Muhammad; Razali, Ili Rabihah; Abdul Kadir, Mohammed Rafiq; Hussain, Rafaqat

2013-01-01

Highlights: ► Phase pure nano-sized sulphur doped hydroxyapatite has been synthesized. ► TEM analysis confirmed formation of needle shaped structure. ► Lattice parameters and cell volume increased with increase in sulphate doping. ► Crystallite size decreased as sulphate content inside the structure increased. ► Degree of crystallinity decreased with increase in sulphate substitution. - Abstract: Inorganic sulphate is required by all mammalian cells to function properly, it is the fourth most abundant anion in the human plasma. Sulphate ions are the major source of sulphur which is considered an important element for sustenance of life as it is present in the essential amino and is required by cells to function properly. In this study we have successfully substituted sulphate ions (SO 4 2− ) into hydroxyapatite (Ca 10 (PO 4 ) 6−x (SO 4 ) x (OH) 2−x ) lattice via ion exchange process with phosphate group. Concentration of SO 4 2− ions was varied between X = 0.05–0.5, using (Ca (NO 3 ) 2 ·4H 2 O), ((NH 4 ) 2 HPO 4 ) and (Na 2 SO 4 ) as starting materials. X-ray diffraction (XRD), Fourier transform IR spectroscopy (FTIR), showed that the substitution of SO 4 2− ions into the lattice resulted in peak broadening and reduced peak height due to the amorphous nature and reduced crystallinity of the resulting HA powder. Transmission electron microscopy (TEM) and field emission electron microscopy (FESEM) analysis confirmed the formation of needle shaped particles of 41 nm size with homogenous and uniform distribution of element within the HA structure

Low temperature synthesis of hydroxyapatite nano-rods by a modified sol-gel technique

International Nuclear Information System (INIS)

Jadalannagari, Sushma; More, Sandeep; Kowshik, Meenal; Ramanan, Sutapa Roy

2011-01-01

Hydroxyapatite (HAp) nano-rods were successfully synthesized by a modified sol-gel method using a solution of CaCl 2 .2H 2 O in water, along with a solution of H 3 PO 4 in triethylamine and NH 4 OH as starting materials. The Ca/P molar ratio was maintained at 1.67. The sol obtained was dried in an oven for 2 days at 100 deg. C after being dialyzed for 12 h. Pellets were made from the crystalline powders and immersed in simulated body fluid (SBF) to check its biocompatibility after 15, 45 and 180 days of immersion. The HAp powders and pellets were characterized by X-Ray Diffraction crystallography (XRD), Fourier transform Infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The HAp nano-rods had an average diameter of 25 nm and length 110-120 nm. Immersion of the HAp pellets in SBF led to the formation of a highly porous interconnecting HAp layer on the surface. The porosity increased with increase in immersion time. Highlights: → Low temperature synthesis of hydroxyapatite nanorods using Ca and P sources and triethylamine. → The synthesis time was only 0.5 hours. → Crystalline material was obtained after drying at 100oC only in air. → SBF studies showed the HAP bodies to be biocompatible.

Study of an ultrasound-based process analytical tool for homogenization of nanoparticulate pharmaceutical vehicles.

Science.gov (United States)

Cavegn, Martin; Douglas, Ryan; Akkermans, Guy; Kuentz, Martin

2011-08-01

There are currently no adequate process analyzers for nanoparticulate viscosity enhancers. This article aims to evaluate ultrasonic resonator technology as a monitoring tool for homogenization of nanoparticulate gels. Aqueous dispersions of colloidal microcrystalline cellulose (MCC) and a mixture of clay particles with xanthan gum were compared with colloidal silicon dioxide in oil. The processing was conducted using a laboratory-scale homogenizing vessel. The study investigated first the homogenization kinetics of the different systems to focus then on process factors in the case of colloidal MCC. Moreover, rheological properties were analyzed offline to assess the structure of the resulting gels. Results showed the suitability of ultrasound velocimetry to monitor the homogenization process. The obtained data were fitted using a novel heuristic model. It was possible to identify characteristic homogenization times for each formulation. The subsequent study of the process factors demonstrated that ultrasonic process analysis was equally sensitive as offline rheological measurements in detecting subtle manufacturing changes. It can be concluded that the ultrasonic method was able to successfully assess homogenization of nanoparticulate viscosity enhancers. This novel technique can become a vital tool for development and production of pharmaceutical suspensions in the future. Copyright © 2011 Wiley-Liss, Inc.

Towards optimization of the silanization process of hydroxyapatite for its use in bone cement formulations

International Nuclear Information System (INIS)

Cisneros-Pineda, Olga G.; Herrera Kao, Wilberth; Loría-Bastarrachea, María I.; Veranes-Pantoja, Yaymarilis; Cauich-Rodríguez, Juan V.; Cervantes-Uc, José M.

2014-01-01

The aim of this work was to provide some fundamental information for optimization of silanization of hydroxyapatite intended for bone cement formulations. The effect of 3-(trimethoxysilyl) propyl methacrylate (MPS) concentration and solvent system (acetone/water or methanol/water mixtures) during HA silanization was monitored by X-ray diffraction (XRD), FTIR spectroscopy and EDX analysis. The effect of silanized HA on the mechanical properties of acrylic bone cements is also reported. It was found that the silanization process rendered hydroxyapatite with lower crystallinity compared to untreated HA. Through EDX, it was observed that the silicon concentration in the HA particles was higher for acetone–water than that obtained for methanol–water system, although the mechanical performance of cements prepared with these particles exhibited the opposite behavior. Taking all these results together, it is concluded that methanol–water system containing MPS at 3 wt.% provides the better results during silanization process of HA. - Highlights: • Effect of MPS concentration and solvents during HA silanization was studied. • Silanization rendered HA has lower crystallinity compared to untreated HA. • Silicon concentration was higher for acetone than that obtained using methanol. • Methanol–water system containing MPS at 3 wt.% provides the better results

Towards optimization of the silanization process of hydroxyapatite for its use in bone cement formulations

Energy Technology Data Exchange (ETDEWEB)

Cisneros-Pineda, Olga G.; Herrera Kao, Wilberth; Loría-Bastarrachea, María I. [Centro de Investigación Científica de Yucatán, A.C., Unidad de Materiales, Calle 43 No. 130, Col. Chuburná de Hidalgo, C.P. 97200 Mérida, Yucatán (Mexico); Veranes-Pantoja, Yaymarilis [Centro de Biomateriales, Universidad de la Habana, Avenida Universidad, s/n, e/G y Ronda, C.P. 10600 C. de La Habana (Cuba); Cauich-Rodríguez, Juan V. [Centro de Investigación Científica de Yucatán, A.C., Unidad de Materiales, Calle 43 No. 130, Col. Chuburná de Hidalgo, C.P. 97200 Mérida, Yucatán (Mexico); Cervantes-Uc, José M., E-mail: manceruc@cicy.mx [Centro de Investigación Científica de Yucatán, A.C., Unidad de Materiales, Calle 43 No. 130, Col. Chuburná de Hidalgo, C.P. 97200 Mérida, Yucatán (Mexico)

2014-07-01

The aim of this work was to provide some fundamental information for optimization of silanization of hydroxyapatite intended for bone cement formulations. The effect of 3-(trimethoxysilyl) propyl methacrylate (MPS) concentration and solvent system (acetone/water or methanol/water mixtures) during HA silanization was monitored by X-ray diffraction (XRD), FTIR spectroscopy and EDX analysis. The effect of silanized HA on the mechanical properties of acrylic bone cements is also reported. It was found that the silanization process rendered hydroxyapatite with lower crystallinity compared to untreated HA. Through EDX, it was observed that the silicon concentration in the HA particles was higher for acetone–water than that obtained for methanol–water system, although the mechanical performance of cements prepared with these particles exhibited the opposite behavior. Taking all these results together, it is concluded that methanol–water system containing MPS at 3 wt.% provides the better results during silanization process of HA. - Highlights: • Effect of MPS concentration and solvents during HA silanization was studied. • Silanization rendered HA has lower crystallinity compared to untreated HA. • Silicon concentration was higher for acetone than that obtained using methanol. • Methanol–water system containing MPS at 3 wt.% provides the better results.

Enhanced mechanical strength of hydroxyapatite nanorods reinforced with polyethylene

International Nuclear Information System (INIS)

Joseph Nathanael, A.; Mangalaraj, D.; Chi Chen, P.; Ponpandian, N.

2011-01-01

Hydroxyapatite (HAp) nanostructures may be an advanced candidate in biomedical applications for an apatite substitute of bone and teeth than other form of HAp. In contrast, well-defined size and shape control in synthesizing HAp nanostructures is always difficult. In this study, hydroxyapatite nanorods (HAp NRs) were prepared by simple hydrothermal method with controlling the reaction time without using any surfactant or templating agents. The nanostructure clearly depicts the growth stages of the HAp NRs by increasing the reaction time. The synthesized HAp has the rod like morphology with uniform size distribution with the aspect ratio of about 8–10. Transmission electron microscopic (TEM) and high resolution TEM (HRTEM) images show that the growth direction of the HAp is parallel to the (001) plane. The interplanar distances measured in segments (fringes) of the HRTEM micrograph were ∼0.35 nm, corresponding to the interplanar spacing of the (002) plane of the hexagonal HAp. X-ray diffraction (XRD) measurements indicate that the improved crystallinity of the HAp by increasing the reaction time. The mechanical studies reveal that the improved tensile strength and the abrasion resistance are observed for the HAp nanorods reinforcing with high molecular weight polyethylene (HMWPE).

Substitution of manganese and iron into hydroxyapatite: Core/shell nanoparticles

International Nuclear Information System (INIS)

Pon-On, Weeraphat; Meejoo, Siwaporn; Tang, I.-Ming

2008-01-01

The bioceramics, hydroxyapatite (HAP), is a material which is biocompatible to the human body and is well suited to be used in hyperthermia applications for the treatment of bone cancer. We investigate the substitution of iron and manganese into the hydroxyapatite to yield ceramics having the empirical formula Ca 9.4 Fe 0.4 Mn 0.2 (PO 4 ) 6 (OH) 2 . The samples were prepared by the co-precipitation method. The formation of the nanocrystallites in the HAP structure as the heating temperatures were raised to obtain a glass-ceramic system are confirmed by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED) and electron spin resonance (ESR). TEM images show the core/shell structure of the nanoparticles, with the core being formed by the ferrites and the shell by the hydroxyapatite. The ED patterns indicate the nanoparticles formed at 500 deg. C have an amorphous structure while the nanoparticles formed at 1000 deg. C are crystalline. ESR spectroscopy indicated that the Fe 3+ ions have a g-factor of 4.23 and the Mn 2+ ions have a g-factor of 2.01. The values of the parameters in the spin Hamiltonian which describes the interaction between the transition metal ions and the Ca 2+ ions, indicate that the Mn 2+ ion substitute into the Ca 2+ sites which are ninefold coordinated, i.e., the Ca(1) sites

Dispersion of nanoparticulate suspensions using self-assembled surfactant aggregates

Science.gov (United States)

Singh, Pankaj Kumar

The dispersion of particles is critical for several industrial applications such as paints, inks, coatings, and cosmetics. Several emerging applications such as abrasives for precision polishing, and drug delivery systems are increasingly relying on nanoparticulates to achieve the desired performance. In the case of nanoparticles, the dispersion becomes more challenging because of the lack of fundamental understanding of dispersant adsorption and interparticle force prediction. Additionally, many of these processes use severe processing environments such as high normal forces (>100 mN/m), high shear forces (>10,000 s -1), and high ionic strengths (>0.1 M). Under such processing conditions, traditionally used dispersants based on electrostatics, and steric force repulsion mechanism may not be adequate. Hence, the development of optimally performing dispersants requires a fundamental understanding of the dispersion mechanism at the atomic/molecular scale. This study explores the use of self-assembled surfactant aggregates at the solid-liquid interface for dispersing nanoparticles in severe processing environments. Surfactant molecules can provide a feasible alternative to polymeric or inorganic dispersants for stabilizing ultrafine particles. The barrier to aggregation in the presence of surfactant molecules was measured using atomic force microscopy. The barrier heights correlated to suspension stability. To understand the mechanism for nanoparticulate suspension stability in the presence of surfactant films, the interface was characterized using zeta potential, contact angle, adsorption, and FT-IR (adsorbed surfactant film structure measurements). The effect of solution conditions such as pH and ionic strength on the suspension stability, and the self-assembled surfactant films was also investigated. It was determined that a transition from a random to an ordered orientation of the surfactant molecules at the interface was responsible for stability of

Development of high strength hydroxyapatite for bone tissue regeneration using nanobioactive glass composites

Science.gov (United States)

Shrivastava, Pragya; Dalai, Sridhar; Sudera, Prerna; Sivam, Santosh Param; Vijayalakshmi, S.; Sharma, Pratibha

2013-02-01

With an increasing demand of biocompatible bone substitutes for the treatment of bone diseases and bone tissue regeneration, bioactive glass composites are being tested to improvise the osteoconductive as well as osteoinductive properties. Nanobioactive glass (nBG) composites, having composition of SiO2 70 mol%, CaO 26 mol % and P2O5 4 mol% were prepared by Freeze drying method using PEG-PPG-PEG co-polymer. Polymer addition improves the mechanical strength and porosity of the scaffold of nBG. Nano Bioactive glass composites upon implantation undergo specific reactions leading to the formation of crystalline hydroxyapatite (HA). This is tested in vitro using Simulated Body Fluid (SBF). This high strength hydroxyapatite (HA) layer acts as osteoconductive in cellular environment, by acting as mineral base of bones, onto which new bone cells proliferate leading to new bone formation. Strength of the nBG composites as well as HA is in the range of cortical and cancellous bone, thus proving significant for bone tissue regeneration substitutes.

Development of high strength hydroxyapatite for bone tissue regeneration using nanobioactive glass composites

International Nuclear Information System (INIS)

Shrivastava, Pragya; Dalai, Sridhar; Vijayalakshmi, S.; Sudera, Prerna; Sivam, Santosh Param; Sharma, Pratibha

2013-01-01

With an increasing demand of biocompatible bone substitutes for the treatment of bone diseases and bone tissue regeneration, bioactive glass composites are being tested to improvise the osteoconductive as well as osteoinductive properties. Nanobioactive glass (nBG) composites, having composition of SiO 2 70 mol%, CaO 26 mol % and P 2 O 5 4 mol% were prepared by Freeze drying method using PEG-PPG-PEG co-polymer. Polymer addition improves the mechanical strength and porosity of the scaffold of nBG. Nano Bioactive glass composites upon implantation undergo specific reactions leading to the formation of crystalline hydroxyapatite (HA). This is tested in vitro using Simulated Body Fluid (SBF). This high strength hydroxyapatite (HA) layer acts as osteoconductive in cellular environment, by acting as mineral base of bones, onto which new bone cells proliferate leading to new bone formation. Strength of the nBG composites as well as HA is in the range of cortical and cancellous bone, thus proving significant for bone tissue regeneration substitutes.

Enhanced bioactivity and biocompatibility of nanostructured hydroxyapatite coating by hydrothermal annealing

International Nuclear Information System (INIS)

Hahn, Byung-Dong; Lee, Jeong-Min; Park, Dong-Soo; Choi, Jong-Jin; Ryu, Jungho; Yoon, Woon-Ha; Choi, Joon-Hwan; Lee, Byoung-Kuk; Kim, Jong-Woo; Kim, Hyoun-Ee; Kim, Seong-Gon

2011-01-01

The crystallinity of hydroxyapatite (HA) coatings prepared by aerosol deposition may be increased by heating in air or low-temperature hydrothermal processing. From the X-ray diffraction and Fourier transform infrared spectroscopy results, it was revealed that the crystallinity of the HA coatings significantly increased after the post-annealing. Transmission electron microscopy showed that the conventional furnace heating induced the substantial growth of the HA crystallites, whereas the hydrothermal treatment did not bring about any remarkable change in the HA crystallite size, which remained below 20 nm. The bioactivity of the HA coatings was estimated by the acellular simulated body fluid immersion test. After immersion for 7 days, newly-precipitated apatite crystals were only observed on the surfaces of the samples hydrothermally treated at 170 and 190 deg. C. In addition, the alkaline phosphatase activity of MC3T3-E1 preosteoblast cells cultured on the hydrothermally treated samples was significantly higher than those on the as-deposited coating and conventional furnace heated samples. The enhanced bioactivity and excellent biological in vitro cellular response of the hydrothermally treated samples were attributed to their nanostructured nature and high degree of crystallinity.

Analysis of the thermoluminescent signal in the hydroxyapatite synthesized by the sol-gel method; Analisis de la senal termoluminiscente en la hidroxiapatita sintetizada por el metodo sol gel

Energy Technology Data Exchange (ETDEWEB)

Mendoza A, D.; Gonzalez, P.R. [ININ, A.P. 18-1027, 11801 Mexico D.F. (Mexico); Lobato, M.; Rubio, E.; Rodriguez L, V. [Fac. de Ingenieria Quimica, BUAP, Av. San Claudio y 18 Sur, Col. San Manuel, 72570 Puebla (Mexico); Custodio, E. [Universidad Juarez Autonoma de Tabasco, DACB, Carr. Cunduacan-Jalpa Km. 1.5, 86680 Tabasco (Mexico)

2004-07-01

The physical properties of the ceramics are related with the chemical bonds and the crystalline structure, because the elements that constitute it can be united by ionic bonds or partially ionic giving a covalent character, this last causes that the outer layer is full of electrons. This property makes that the ceramic ones become interesting materials for thermoluminescent applications, as it demonstrates through the recent works presented on the hydroxyapatite that is a ceramic biomaterials that has shown an interesting thermoluminescent signal when being exposed to gamma radiation. In this sense, this work presents the thermoluminescent signal analysis induced by the UV and gamma radiation in a particular type of hydroxyapatite synthesized by sol gel method in which the temperature synthesis is varied. The final thermoluminescent sensitivity of materials is correlated with the crystalline degree, which is analysed through X-ray diffraction. (Author)

Microwave assisted synthesis of nano sized sulphate doped hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Alshemary, Ammar Z.; Goh, Yi-Fan; Akram, Muhammad; Razali, Ili Rabihah [Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor Darul Ta’zim (Malaysia); Abdul Kadir, Mohammed Rafiq [Medical Implant Technology Group, Faculty of Biomedical Engineering and Health Science, Universiti Teknologi Malaysia,81310 UTM Skudai, Johor Darul Ta’zim (Malaysia); Hussain, Rafaqat, E-mail: rafaqat@kimia.fs.utm.my [Ibnu Sina Institute for Fundamental Science Studies, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor DarulTa’zim (Malaysia)

2013-06-01

Highlights: ► Phase pure nano-sized sulphur doped hydroxyapatite has been synthesized. ► TEM analysis confirmed formation of needle shaped structure. ► Lattice parameters and cell volume increased with increase in sulphate doping. ► Crystallite size decreased as sulphate content inside the structure increased. ► Degree of crystallinity decreased with increase in sulphate substitution. - Abstract: Inorganic sulphate is required by all mammalian cells to function properly, it is the fourth most abundant anion in the human plasma. Sulphate ions are the major source of sulphur which is considered an important element for sustenance of life as it is present in the essential amino and is required by cells to function properly. In this study we have successfully substituted sulphate ions (SO{sub 4}{sup 2−}) into hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6−x}(SO{sub 4}){sub x}(OH){sub 2−x}) lattice via ion exchange process with phosphate group. Concentration of SO{sub 4}{sup 2−} ions was varied between X = 0.05–0.5, using (Ca (NO{sub 3}){sub 2}·4H{sub 2}O), ((NH{sub 4}){sub 2}HPO{sub 4}) and (Na{sub 2}SO{sub 4}) as starting materials. X-ray diffraction (XRD), Fourier transform IR spectroscopy (FTIR), showed that the substitution of SO{sub 4}{sup 2−} ions into the lattice resulted in peak broadening and reduced peak height due to the amorphous nature and reduced crystallinity of the resulting HA powder. Transmission electron microscopy (TEM) and field emission electron microscopy (FESEM) analysis confirmed the formation of needle shaped particles of 41 nm size with homogenous and uniform distribution of element within the HA structure.

Characterization of Mg-containing hydroxyapatites synthesized by combustion method

Science.gov (United States)

Kaygili, Omer; Keser, Serhat; Bulut, Niyazi; Ates, Tankut

2018-05-01

In the present paper, Mg-substituted hydroxyapatites with the morphology, composed of the stacked plate- and rod-like structures, were prepared at the temperature of 600 °C by combustion method using glycerine as a fuel. A significant decrease in the crystallite size values calculated for both Scherrer and Williamson-Hall methods is found. The crystallinity, lattice parameter of a, stress and anisotropic energy density values decreased by adding of Mg, whereas the lattice strain increased. The amount of HAp phase decreases with increasing amount of Mg and the β-tricalcium phosphate content increases. Mg incorporation the apatitic structure was detected. Depending on the increase in Mg content, Ca-deficiency was observed.

Low temperature synthesis and characterization of carbonated hydroxyapatite nanocrystals

Science.gov (United States)

Anwar, Aneela; Asghar, Muhammad Nadeem; Kanwal, Qudsia; Kazmi, Mohsin; Sadiqa, Ayesha

2016-08-01

Carbonate substituted hydroxyapatite (CHA) nanorods were synthesized via coprecipitation method from aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate (with urea as carbonate ion source) in the presence of ammonium hydroxide solution at 70 °C at the conditions of pH 11. The obtained powders were physically characterized using transmission electron microscopy (TEM), X-ray powder diffraction analysis (XRD), and FTIR and Raman spectroscopy. The particle size was evaluated by Dynamic light scattering (DLS). The chemical structural analysis of as prepared sample was performed using X-ray photoelectron spectroscopy (XPS). After ageing for 12 h, and heat treatment at 1000 °C for 1 h, the product was obtained as highly crystalline nanorods of CHA.

Synthesis and characterization of hydroxyapatite-gelatine composite materials for orthopaedic application

International Nuclear Information System (INIS)

Yanovska, A.; Kuznetsov, V.; Stanislavov, A.; Husak, E.; Pogorielov, M.; Starikov, V.; Bolshanina, S.; Danilchenko, S.

2016-01-01

The composite materials based on hydroxyapatite (HA) and gelatine (Gel) with addition of silver and zirconium oxide were obtained. The study investigates a combination of low powered ultrasonic irradiation and low concentration of gelatine in the co-precipitation synthesis. These composites have different weight ratios of organic/inorganic components and may be synthesized in two ways: simple mixing and co-precipitation. Both of which were compared. The estimation of porosity, in vivo testing, surface morphology and phase composition as well as the IR-analysis were provided. Hydroxyapatite was the main crystalline phase in obtained composites. While around powdered HA-Gel composite the connective tissue capsule is formed without bone tissue formation, HA-Gel-Ag porous composite implantation leads to formation of new bone tissue and activation of cell proliferation. Addition of silver ions into composite material allows decreasing inflammation on the first stage of implantation and has positive effect on bone tissue formation. Some of the obtained composite materials containing silver or ZrO_2 are biocompatible. bio-resorbable and osteoconductive with high level of porosity (75–85%). - Highlights: • Hydroxyapatite-gelatine composites with addition of Ag"+ and ZrO_2 were obtained. • Composites were synthesized in two ways: simple mixing and co-precipitation. • Co-precipitation synthesis combined ultrasonic treatment and low concentration of gelatine. • Obtained composites have different weight ratios of organic/inorganic components. • Some composites are osteoconductive and all of them have high level of porosity (75–85%).

Ostrich eggshell as calcium source for the synthesis of hydroxyapatite and hydroxyapatite partially substituted with zinc

International Nuclear Information System (INIS)

Ferreira, J.R.M.; Louro, L.H.L.; Costa, A.M.; Silva, M.H. Prado da; Campos, J.B. de

2016-01-01

In the present study, hydroxyapatite and Zn-substituted hydroxyapatite powders were synthesized using ostrich eggshell as a calcium source. The samples were analyzed by scanning electron microscopy with field emission gun, and X-ray diffraction (XRD) to identify the present phases, and X-ray fluorescence spectroscopy for quantitative chemical analysis of the synthesized and heat treated powders. The Fourier transform infrared spectroscopy technique was used before and after heat treatments at 700, 900 and 1100 °C in order to identify the functional groups present, as an additional technique to the XRD analysis. The results presented in this study represent a promising method for synthesis of hydroxyapatite and hydroxyapatite partially substituted with zinc, since the results showed no undesirable phases or impurities in the produced powders. It was observed that Zn-substituted hydroxyapatite showed higher thermal stability, when compared to pure hydroxyapatite. (author)

Ostrich eggshell as calcium source for the synthesis of hydroxyapatite and hydroxyapatite partially substituted with zinc

Energy Technology Data Exchange (ETDEWEB)

Ferreira, J.R.M.; Louro, L.H.L.; Costa, A.M.; Silva, M.H. Prado da [Instituto Militar de Engenharia (IME), Rio de Janeiro, RJ (Brazil); Campos, J.B. de, E-mail: josericardo@r-crio.com, E-mail: louro@ime.eb.br, E-mail: andrea@r-crio.com, E-mail: brantjose@gmail.com, E-mail: marceloprado@ime.eb.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil)

2016-10-15

In the present study, hydroxyapatite and Zn-substituted hydroxyapatite powders were synthesized using ostrich eggshell as a calcium source. The samples were analyzed by scanning electron microscopy with field emission gun, and X-ray diffraction (XRD) to identify the present phases, and X-ray fluorescence spectroscopy for quantitative chemical analysis of the synthesized and heat treated powders. The Fourier transform infrared spectroscopy technique was used before and after heat treatments at 700, 900 and 1100 °C in order to identify the functional groups present, as an additional technique to the XRD analysis. The results presented in this study represent a promising method for synthesis of hydroxyapatite and hydroxyapatite partially substituted with zinc, since the results showed no undesirable phases or impurities in the produced powders. It was observed that Zn-substituted hydroxyapatite showed higher thermal stability, when compared to pure hydroxyapatite. (author)

Comparative physical, chemical and biological assessment of simple and titanium-doped ovine dentine-derived hydroxyapatite coatings fabricated by pulsed laser deposition

Science.gov (United States)

Duta, L.; Mihailescu, N.; Popescu, A. C.; Luculescu, C. R.; Mihailescu, I. N.; Çetin, G.; Gunduz, O.; Oktar, F. N.; Popa, A. C.; Kuncser, A.; Besleaga, C.; Stan, G. E.

2017-08-01

We report on the synthesis by Pulsed Laser Deposition of simple and Ti doped hydroxyapatite thin films of biological (ovine dentine) origin. Detailed physical, chemical, mechanical and biological investigations were performed. Morphological examination of films showed a surface composed of spheroidal particulates, of micronic size. Compositional analyses pointed to the presence of typical natural doping elements of bone, along with a slight non-stoichiometry of the deposited films. Structural investigations proved the monophasic hydroxyapatite nature of both simple and Ti doped films. Ti doping of biological hydroxyapatite induced an overall downgrade of the films crystallinity together with an increase of the films roughness. It is to be emphasized that bonding strength values measured at film/Ti substrate interface were superior to the minimum value imposed by International Standards regulating the load-bearing implant coatings. In vitro tests on Ti doped structures, compared to simple ones, revealed excellent biocompatibility in human mesenchymal stem cell cultures, a higher proliferation rate and a good cytocompatibility. The obtained results aim to elucidate the overall positive role of Ti doping on the hydroxyapatite films performance, and demonstrate the possibility to use this novel type of coatings as feasible materials for future implantology applications.

Ostrich eggshell as calcium source for the synthesis of hydroxyapatite and hydroxyapatite partially substituted with zinc

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J. R. M. Ferreira

Full Text Available Abstract In the present study, hydroxyapatite and Zn-substituted hydroxyapatite powders were synthesized using ostrich eggshell as a calcium source. The samples were analyzed by scanning electron microscopy with field emission gun, and X-ray diffraction (XRD to identify the present phases, and X-ray fluorescence spectroscopy for quantitative chemical analysis of the synthesized and heat treated powders. The Fourier transform infrared spectroscopy technique was used before and after heat treatments at 700, 900 and 1100 °C in order to identify the functional groups present, as an additional technique to the XRD analysis. The results presented in this study represent a promising method for synthesis of hydroxyapatite and hydroxyapatite partially substituted with zinc, since the results showed no undesirable phases or impurities in the produced powders. It was observed that Zn-substituted hydroxyapatite showed higher thermal stability, when compared to pure hydroxyapatite.

Comparative study between bioapatite and synthetic hydroxyapatite obtained by chemical precipitation and mechanochemical synthesis

International Nuclear Information System (INIS)

Quispe M, J.; Moreno, M.; Montano, J.; Pillaca, M.; Guzman, A.; Cavero, A.; Arce, M.

2009-01-01

A comparative study between the inorganic component of a human bone tissue with respect of apatite synthesized by chemical precipitation, mechanochemical synthesis and a sample of commercial hidroxyapatite are shown. The samples were studied by X-ray diffraction, atomic absorption spectroscopy and Fourier transform infrared spectroscopy. The results show similar structural characteristics among all samples identifying that sample prepared by mechanochemical synthesis is a kind of hydroxyapatite which has substitutions of carbonate in its crystalline structure, similar to the inorganic component of bone tissue. (author).

Synthesis and Characterization of Hydroxyapatite/Fullerenol Nanocomposites.

Science.gov (United States)

Djordjevic, Aleksandar; Ignjatovic, Nenad; Seke, Mariana; Jovic, Danica; Uskokovic, Dragan; Rakocevic, Zlatko

2015-02-01

Fullerenols are polyhydroxylated, water soluble derivatives of fullerene C60, with potential application in medicine as diagnostic agents, antioxidants or nano drug carriers. This paper describes synthesis and physical characterization of a new nanocomposite hydroxyapatite/fullerenol. Surface of the nanocomposite hydroxyapatite/fullerenol is inhomogeneous with the diameter of the particles in the range from 100 nm to 350 nm. The ζ potential of this nanocomposite is ten times lower when compared to hydroxyapatite. Surface phosphate groups of hydroxyapatite are prone to forming hydrogen bonds, when in close contact with hydroxyl groups, which could lead to formation of hydrogen bonds between hydroxyapatite and hydroxyl groups of fullerenol. The surface of hydroxyapatite particles (-2.5 mV) was modified by fullerenol particles, as confirmed by the obtained ζ potential value of the nanocomposite biomaterial hydroxyapatite/fullerenol (-25.0 mV). Keywords: Hydroxyapatite, Fullerenol, Nanocomposite, Surface Analysis.

Effects of fluoridation of porcine hydroxyapatite on osteoblastic activity of human MG63 cells

International Nuclear Information System (INIS)

Li, Zhipeng; Huang, Baoxin; Mai, Sui; Wu, Xiayi; Zhang, Hanqing; Qiao, Wei; Luo, Xin; Chen, Zhuofan

2015-01-01

Biological hydroxyapatite, derived from animal bones, is the most widely used bone substitute in orthopedic and dental treatments. Fluorine is the trace element involved in bone remodeling and has been confirmed to promote osteogenesis when administered at the appropriate dose. To take advantage of this knowledge, fluorinated porcine hydroxyapatite (FPHA) incorporating increasing levels of fluoride was derived from cancellous porcine bone through straightforward chemical and thermal treatments. Physiochemical characteristics, including crystalline phases, functional groups and dissolution behavior, were investigated on this novel FPHA. Human osteoblast-like MG63 cells were cultured on the FPHA to examine cell attachment, cytoskeleton, proliferation and osteoblastic differentiation for in vitro cellular evaluation. Results suggest that fluoride ions released from the FPHA play a significant role in stimulating osteoblastic activity in vitro, and appropriate level of fluoridation (1.5 to 3.1 atomic percents of fluorine) for the FPHA could be selected with high potential for use as a bone substitute. (paper)

Room temperature ferromagnetism in Eu-doped ZnO nanoparticulate powders prepared by combustion reaction method

International Nuclear Information System (INIS)

Franco, A.; Pessoni, H.V.S.; Soares, M.P.

2014-01-01

Nanoparticulate powders of Eu-doped ZnO with 1.0, 1.5, 2.0 and 3.0 at% Eu were synthesized by combustion reaction method using zinc nitrate, europium nitrate and urea as fuel without subsequent heat treatments. X-ray diffraction patterns (XRD) of all samples showed broad peaks consistent with the ZnO wurtzite structure. The absence of extra reflections in the diffraction patterns ensures the phase purity, except for x=0.03 that exhibits small reflection corresponding to Eu 2 O 3 phase. The average crystallite size determined from the most prominent (1 0 1) peak of the diffraction using Scherrer's equation was in good agreement with those determined by transmission electron microscopy (TEM); being ∼26 nm. The magnetic properties measurements were performed using a vibrating sample magnetometer (VSM) in magnetic fields up to 2.0 kOe at room temperature. The hysteresis loops, typical of magnetic behaviors, indicating that the presence of an ordered magnetic structure can exist in the Eu-doped ZnO wurtzite structure at room temperature. The room temperature ferromagnetism behavior increases with the Eu 3+ doping concentration. All samples exhibited the same Curie temperature (T C ) around ∼726 K, except for x=0.01; T C ∼643 K. High resolution transmission electron microscopy (HRTEM) images revealed defects/strain in the lattice and grain boundaries of Eu-doped ZnO nanoparticulate powders. The origin of room temperature ferromagnetism in Eu-doped ZnO nanoparticulate powders was discussed in terms of these defects, which increase with the Eu 3+ doping concentration. - Highlights: • Room-temperature ferromagnetism. • Structural and magnetic properties of nanoparticulate powders of Zn 1−x Eu x O. • Combustion reaction method

Preparation and characterization of nano-hydroxyapatite within chitosan matrix

International Nuclear Information System (INIS)

Rogina, A.; Ivanković, M.; Ivanković, H.

2013-01-01

Nano-composites that show some features of natural bone both in composition and in microstructure have been prepared by in situ precipitation method. Apatite phase has been prepared from cost-effective precursors (calcite and urea phosphate) within chitosan (CS) matrix dissolved in aqueous acetic acid solution. The compositional and morphological properties of composites were studied by means of Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) thermogravimetric analysis (TGA) and transmission electron microscopy (TEM). Depending on the reaction conditions (temperature, reaction time, glucose addition and pH control) in addition to hydroxyapatite (HA) as a major phase, octacalcium hydrogen phosphate pentahydrate (OCP) and dicalcium phosphate anhydrate (DCPD) were formed as shown by XRD and FTIR. Crystallite lengths of precipitated HA estimated by Scherrer's equation were between 20 and 30 nm. A fibrous morphology (∼ 400 nm) of HA observed by TEM indicates that HA nucleates on chitosan chains. - Highlights: • Nano-hydroxyapatite (HA) was prepared by in situ precipitation within chitosan hydrogels and colloidal chitosan solution. • pH control was regulated by ammonia and urea degradation. • In situ urea degradation provides homogenous HA formation. • TEM imaging indicates fibrous morphology of HA with crystalline size of 400 nm. • Glucose addition and temperature variation affect inorganic phase formation

Similar healthy osteoclast and osteoblast activity on nanocrystalline hydroxyapatite and nanoparticles of tri-calcium phosphate compared to natural bone

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MacMillan AK

2014-12-01

Full Text Available Adam K MacMillan,1 Francis V Lamberti,1 Julia N Moulton,2 Benjamin M Geilich,2 Thomas J Webster2,3 1RTI Surgical, Alachua, FL, USA; 2Department of Chemical Engineering, Northeastern University, Boston, MA, USA; 3Center of Excellence for Advanced Materials Research, King Abdulaziz University, Jeddah, Saudi Arabia Abstract: While there have been numerous studies to determine osteoblast (bone forming cell functions on nanocrystalline compared to micron crystalline ceramics, there have been few studies which have examined osteoclast activity (including tartrate-resistant acid phosphatase, formation of resorption pits, size of resorption pits, and receptor activator of nuclear factor κB [RANK]. This is despite the fact that osteoclasts are an important part of maintaining healthy bone since they resorb bone during the bone remodeling process. Moreover, while it is now well documented that bone formation is enhanced on nanoceramics compared to micron ceramics, some have pondered whether osteoblast functions (such as osteoprotegerin and RANK ligand [RANKL] are normal (ie, non-diseased on such materials compared to natural bone. For these reasons, the objective of the present in vitro study was to determine various functions of osteoclasts and osteoblasts on nanocrystalline and micron crystalline hydroxyapatite as well as tri-calcium phosphate materials and compare such results to cortical and cancellous bone. Results showed for the first time similar osteoclast activity (including tartrate-resistant acid phosphatase, formation of resorption pits, size of resorption pits, and RANK and osteoblast activity (osteoprotegerin and RANKL on nanocrystalline hydroxyapatite compared to natural bone, whereas osteoclast and osteoblast functions on micron crystalline versions of these ceramics were much different than natural bone. In this manner, this study provides additional evidence that nanocrystalline calcium phosphates can serve as suitable synthetic

In situ synthesis carbonated hydroxyapatite layers on enamel slices with acidic amino acids by a novel two-step method.

Science.gov (United States)

Wu, Xiaoguang; Zhao, Xu; Li, Yi; Yang, Tao; Yan, Xiujuan; Wang, Ke

2015-09-01

In situ fabrication of carbonated hydroxyapatite (CHA) remineralization layer on an enamel slice was completed in a novel, biomimetic two-step method. First, a CaCO3 layer was synthesized on the surface of demineralized enamel using an acidic amino acid (aspartic acid or glutamate acid) as a soft template. Second, at the same concentration of the acidic amino acid, rod-like carbonated hydroxyapatite was produced with the CaCO3 layer as a sacrificial template and a reactant. The morphology, crystallinity and other physicochemical properties of the crystals were characterized using field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrometry (FTIR), X-ray diffraction (XRD) and energy-dispersive X-ray analysis (EDAX), respectively. Acidic amino acid could promote the uniform deposition of hydroxyapatite with rod-like crystals via absorption of phosphate and carbonate ions from the reaction solution. Moreover, compared with hydroxyapatite crystals coated on the enamel when synthesized by a one-step method, the CaCO3 coating that was synthesized in the first step acted as an active bridge layer and sacrificial template. It played a vital role in orienting the artificial coating layer through the template effect. The results show that the rod-like carbonated hydroxyapatite crystals grow into bundles, which are similar in size and appearance to prisms in human enamel, when using the two-step method with either aspartic acid or acidic glutamate (20.00 mmol/L). Copyright © 2015 Elsevier B.V. All rights reserved.

Ellipsometric analysis and optical absorption characterization of gallium phosphide nanoparticulate thin film

Science.gov (United States)

Zhang, Qi-Xian; Wei, Wen-Sheng; Ruan, Fang-Ping

2011-04-01

Gallium phosphide (GaP) nanoparticulate thin films were easily fabricated by colloidal suspension deposition via GaP nanoparticles dispersed in N,N-dimethylformamide. The microstructure of the film was performed by x-ray diffraction, high resolution transmission electron microscopy and field emission scanning electron microscopy. The film was further investigated by spectroscopic ellipsometry. After the model GaP+void|SiO2 was built and an effective medium approximation was adopted, the values of the refractive index n and the extinction coefficient k were calculated for the energy range of 0.75 eV-4.0 eV using the dispersion formula in DeltaPsi2 software. The absorption coefficient of the film was calculated from its k and its energy gaps were further estimated according to the Tauc equation, which were further verified by its fluorescence spectrum measurement. The structure and optical absorption properties of the nanoparticulate films are promising for their potential applications in hybrid solar cells.

Electrophoretic deposition of composite hydroxyapatite-chitosan coatings

International Nuclear Information System (INIS)

Pang Xin; Zhitomirsky, Igor

2007-01-01

Cathodic electrophoretic deposition has been utilized for the fabrication of composite hydroxyapatite-chitosan coatings on 316L stainless steel substrates. The addition of chitosan to the hydroxyapatite suspensions promoted the electrophoretic deposition of the hydroxyapatite nanoparticles and resulted in the formation of composite coatings. The obtained coatings were investigated by X-ray diffraction, thermogravimetric and differential thermal analysis, scanning and transmission electron microscopy, potentiodynamic polarization measurements, and electrochemical impedance spectroscopy. It was shown that the deposit composition can be changed by a variation of the chitosan or hydroxyapatite concentration in the solutions. Experimental conditions were developed for the fabrication of hydroxyapatite-chitosan nanocomposites containing 40.9-89.8 wt.% hydroxyapatite. The method enabled the formation of adherent and uniform coatings of thicknesses up to 60 μm. X-ray studies revealed that the preferred orientation of the hydroxyapatite nanoparticles in the chitosan matrix increases with decreasing hydroxyapatite content in the composite coatings. The obtained coatings provided the corrosion protection for the 316L stainless steel substrates

A simple and rapid method to graft hydroxyapatite on carbon nanotubes

International Nuclear Information System (INIS)

Neelgund, Gururaj M.; Olurode, Kehinde; Luo Zhiping; Oki, Aderemi

2011-01-01

Herein a simple and effective approach is introduced to functionalize single walled carbon nanotubes (SWCNTs) by in-situ grafting of hydroxyapatite (HA). The pristine SWCNTs were chemically activated through introduction of carboxylic groups on their surfaces by refluxing in the mixture of H 2 SO 4 and HNO 3 . The resulting carboxylated SWCNTs were further utilized for grafting of HA. The Fourier transform infrared and Raman spectroscopic studies demonstrated the formation of HA and its grafting over SWCNTs. The phase composition of HA and existence Ca 2+ and PO 4 3- ions were studied using X-ray diffraction and energy dispersive X-ray analyses, respectively. The surface morphology of functionalized SWCNTs was analyzed using scanning electron microscopy and transmission electron microscopy. Thermogravimetric analysis confirmed the existence of HA on SWCNTs by exhibiting different thermogram for pure HA and functionalized SWCNTs. Overall, this method produced uniform grafting of low crystalline HA on carboxylated SWCNTs with strong interfacial bonding. - Graphical abstract: A facile approach is demonstrated for effective functionalization of single walled carbon nanotubes (SWCNTs) by in-situ grafting of hydroxyapatite (HA) to improve hydrophilicity and biocompatibility of SWCNTs. This method produced uniform grafting of low crystalline HA on carboxylated SWCNTs with strong interfacial bonding. Research highlights: → This method is facile and effective to graft HA on SWCNTs. → As f-SWCNTs is a promising biomaterial to use without any further processing → This technique is economic, easy to repeat and can be optimized for mass production. → Ratio of Ca to P in f-SWCNTs was 1.65, which is near to ratio present in bone tissue.

A simple and rapid method to graft hydroxyapatite on carbon nanotubes

Energy Technology Data Exchange (ETDEWEB)

Neelgund, Gururaj M.; Olurode, Kehinde [Department of Chemistry, Prairie View A and M University, Prairie View, TX 77446 (United States); Luo Zhiping [Microscopy and Imaging Center, Materials Science and Engineering, Texas A and M University, College Station TX 77843 (United States); Oki, Aderemi, E-mail: aroki@pvamu.edu [Department of Chemistry, Prairie View A and M University, Prairie View, TX 77446 (United States)

2011-10-10

Herein a simple and effective approach is introduced to functionalize single walled carbon nanotubes (SWCNTs) by in-situ grafting of hydroxyapatite (HA). The pristine SWCNTs were chemically activated through introduction of carboxylic groups on their surfaces by refluxing in the mixture of H{sub 2}SO{sub 4} and HNO{sub 3}. The resulting carboxylated SWCNTs were further utilized for grafting of HA. The Fourier transform infrared and Raman spectroscopic studies demonstrated the formation of HA and its grafting over SWCNTs. The phase composition of HA and existence Ca{sup 2+} and PO{sub 4}{sup 3-} ions were studied using X-ray diffraction and energy dispersive X-ray analyses, respectively. The surface morphology of functionalized SWCNTs was analyzed using scanning electron microscopy and transmission electron microscopy. Thermogravimetric analysis confirmed the existence of HA on SWCNTs by exhibiting different thermogram for pure HA and functionalized SWCNTs. Overall, this method produced uniform grafting of low crystalline HA on carboxylated SWCNTs with strong interfacial bonding. - Graphical abstract: A facile approach is demonstrated for effective functionalization of single walled carbon nanotubes (SWCNTs) by in-situ grafting of hydroxyapatite (HA) to improve hydrophilicity and biocompatibility of SWCNTs. This method produced uniform grafting of low crystalline HA on carboxylated SWCNTs with strong interfacial bonding. Research highlights: {yields} This method is facile and effective to graft HA on SWCNTs. {yields} As f-SWCNTs is a promising biomaterial to use without any further processing {yields} This technique is economic, easy to repeat and can be optimized for mass production. {yields} Ratio of Ca to P in f-SWCNTs was 1.65, which is near to ratio present in bone tissue.

Rapid Obtaining of Nano-Hydroxyapatite Bioactive Films on NiTi Shape Memory Alloy by Electrodeposition Process

Science.gov (United States)

Lobo, A. O.; Otubo, J.; Matsushima, J. T.; Corat, E. J.

2011-07-01

Nano-hydroxyapatite (n-HA) crystalline films have been developed in this study by electrodeposition method on NiTi shape memory alloy (SMA). The electrodeposition of the n-HA films was carried out using 0.042 mol/L Ca(NO3)2 · 4H2O + 0.025 mol/L (NH4) · 2HPO4 electrolytes by applying a constant potential of -2.0 V for 120 min and keeping the solution temperature at 70 °C. The characterization of n-HA films is of special importance since bioactive properties related to n-HA have been directly identified with its specific composition and crystalline structure. AFM, XRD, EDX, FEG-SEM and Raman spectroscopy shows a homogeneous film, with high crystallinity, special composition, and bioactivity properties (Ca/P = 1.93) of n-HA on NiTi SMA surfaces. The n-HA coating with special structure would benefit the use of NiTi alloy in orthopedic applications.

Particle morphology of hydroxyapatite and its influence on the properties of biocomposite plasma coatings

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Melnikova I.P.

2013-09-01

Full Text Available The purpose of the article is to identify patterns of change in the properties of biocompatible coatings during modernization of its structure by changing the morphology and crystallinity of the starting powder particles of hydroxyapatite (HA for agglomeration and subsequent grinding. Material and methods. We investigated the morphology, degree of crystallinity and internal tension in HA powder with a particle size of 40-90 microns in the initial state and after the agglomeration process and structure piasmasprayed HA coatings application methods ray analysis (XRF and XRD on DRON-3, infrared spectroscopy (FT-IR spectrometer Nicolet 6700, optical (MIM-8 and atomic force microscopy (SMM-2000, the laser microprobe (Spectrum 2000. Results: It was shown that change in particle morphology HA agglomerated and subsequently grinding increases the uniformity of the porous structure, its crystallinity, reduce internal stresses developing surface morphology of the coating and its nanostructuring. Conclusion. It is recommended for the improvement of characteristics of the porous structure (uniformity, strength, adhesion, and the surface morphology of implant to use agglomerating starting powders and their subsequent grinding.

Spectral luminescent properties of bacteriochlorin and aluminum phthalocyanine nanoparticles as hydroxyapatite implant surface coating

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Yu. S. Maklygina

2016-01-01

Full Text Available The development and the spectral research of unique coating as crystalline nanoparticles of IR photosensitizers were performed for the creation of hydroxyapatite implants with photobactericidal properties. It has been proved that by the interaction of nanoparticles covering implant with the polar solvent, which simulates the interaction of the implant with the biocomponents in vivo (fast proliferating and with immunocompetent cells, photosensitizers nanoparticles change the spectroscopic properties, becoming fluorescent and phototoxic. Thus, the developed coating based on crystalline photosensitizer nanoparticles with studied specific properties should have antibacterial, anti-inflammatory effect by the photodynamic treatment in the near implant area. This research opens the prospect of the local prevention of inflammatory and autoimmune reactions in the area of implantation. The results of the study suggest a promising this technology in order to create implants with photobactericidal properties.

Preparation and characterization of gelatin–hydroxyapatite composite microspheres for hard tissue repair

International Nuclear Information System (INIS)

Chao, Shao Ching; Wang, Ming-Jia; Pai, Nai-Su; Yen, Shiow-Kang

2015-01-01

Gelatin–hydroxyapatite composite microspheres composed of 21% gelatin (G) and 79% hydroxyapatite (HA) with uniform morphology and controllable size were synthesized from a mixed solution of Ca(NO 3 ) 2 , NH 4 H 2 PO 4 and gelatin by a wet-chemical method. Material analyses such as X-ray diffraction (XRD), scanning/transmission electron microscopy examination (SEM/TEM) and inductively coupled plasma-mass spectroscopy (ICP-MS) were used to characterize G–HA microspheres by analyzing their crystalline phase, microstructure, morphology and composition. HA crystals precipitate along G fibers to form nano-rods with diameters of 6–10 nm and tangle into porous microspheres after blending. The cell culture indicates that G–HA composite microspheres without any toxicity could enhance the proliferation and differentiation of osteoblast-like cells. In a rat calvarial defect model, G–HA bioactive scaffolds were compared with fibrin glue (F) and Osteoset® Bone Graft Substitute (OS) for their capacity of regenerating bone. Four weeks post-implantation, new bone, mineralization, and expanded blood vessel area were found in G–HA scaffolds, indicating greater osteoconductivity and bioactivity than F and OS. - Highlights: • G–HA composite microspheres were prepared by hydroxyapatite and gelatin. • In vitro tests indicated that the G–HA microspheres were biocompatible and bioactive. • In in vitro tests, G–HA microspheres could be applied in hard tissue engineering. • G–HA had healed the bone defect and provides a high proportion of surface area to open space

TSDC and impedance spectroscopy measurements on hydroxyapatite, β-tricalcium phosphate and hydroxyapatite/β-tricalcium phosphate biphasic bioceramics

Science.gov (United States)

Prezas, P. R.; Melo, B. M. G.; Costa, L. C.; Valente, M. A.; Lança, M. C.; Ventura, J. M. G.; Pinto, L. F. V.; Graça, M. P. F.

2017-12-01

Bone grafting and surgical interventions related with orthopaedic disorders consist in a big business, generating large revenues worldwide every year. There is a need to replace the biomaterials that currently still dominate this market, i.e., autografts and allografts, due to their disadvantages, such as limited availability, need for additional surgeries and diseases transmission possibilities. The most promising replacement materials are biomaterials with bioactive properties, such as the calcium phosphate-based bioceramics group. The bioactivity of these materials, i.e., the rate at which they promote the growth and directly bond with the new host biological bone, can be enhanced through their electrical polarization. In the present work, the electrical polarization features of pure hydroxyapatite (Hap), pure β-tricalcium phosphate (β-TCP) and biphasic hydroxyapatite/β-tricalcium phosphate composites (HTCP) were analyzed by measuring thermally stimulated depolarization currents (TSDC). The samples were thermoelectrically polarized at 500 °C under a DC electric field with a magnitude of 5 kV/cm. The biphasic samples were also polarized under electric fields with different magnitudes: 2, 3, 4 and 5 kV/cm. Additionally, the depolarization processes detected in the TSDC measurements were correlated with dielectric relaxation processes observed in impedance spectroscopy (IS) measurements. The results indicate that the β-TCP crystalline phase has a considerable higher ability to store electrical charge compared with the Hap phase. This indicates that it has a suitable composition and structure for ionic conduction and establishment of a large electric charge density, providing great potential for orthopaedic applications.

Synthesis and study of the synthetic hydroxyapatite doped with aluminum

Science.gov (United States)

Goldberg, M.; Smirnov, V.; Antonova, O.; Konovalov, A.; Fomina, A.; Komlev, V. S.; Barinov, S.; Rodionov, A.; Gafurov, M.; Orlinskii, S.

2018-05-01

Powders of synthetic hydroxyapatite doped with aluminium (Al) ions in concentrations 0 and 20 mol. % were synthesized by the precipitation method from the nitrate solutions and investigated by atomic emission spectrometry with inductively coupled plasma (AES-ICP), X-ray diffraction (XRD), scanning electron microscopy (SEM), gas absorption and conventional electron paramagnetic resonance (EPR). It is shown that for the chosen synthesis route an introduction of Al provokes formation of highly anisotropic phase, leads to the decrease in the crystallinity while no significant changes in the EPR spectra of the radiation-induced defects is observed. The results could be used for understanding the structural transformations with Al doping of the mineralized materials for geological and biomedical applications.

Coating of the orthopaedic titanium alloys with sol-gel derived hydroxyapatite

International Nuclear Information System (INIS)

Milev, A.; Green, D.; Chai, C.S.; Ben-Nissan, B.

1999-01-01

Hydroxyapatite (HAp) is known to be both biocompatible and bioactive material, however, due to its poor mechanical properties and design limitations is not suitable for applying as a load bearing implant. This could be overcome by using appropriate metallic substrates covered with HAp, derived via different techniques. These coatings allow improved adhesion strength of the load bearing substrate to the bone, resulting in shorter healing periods as well as predictable behaviour of the implant for longer periods of time. There are different techniques of producing HAp appropriate for coating purposes. Due to the small particle size of the grains derived, sol-gel route is preferable where lower sintering temperatures are of primary importance. For better adhesion between substrate and hydroxyapatite coating, the surface of titanium substrate, in this study, was converted to titanium nitride and/or oxynitride. Sintering temperatures of 900 deg C have been used for producing crystalline HAp coatings. The control of sol-gel solutions and the analysis of the coatings were carried out using XRD, SEM and DTA techniques. Results obtained indicate high quality HAp coatings can be produced on titanium substrates especially with complex shapes that benefits over the other coating methods

Collagen immobilized PVA hydrogel-hydroxyapatite composites prepared by kneading methods as a material for peripheral cuff of artificial cornea

International Nuclear Information System (INIS)

Kobayashi, Hisatoshi; Kato, Masabumi; Taguchi, Tetsushi; Ikoma, Toshiyuki; Miyashita, Hideyuki; Shimmura, Shigeto; Tsubota, Kazuo; Tanaka, Junzo

2004-01-01

In order to achieve the firm fixation of the artificial cornea to host tissues, composites of collagen-immobilized poly(vinyl alcohol) hydrogel with hydroxyapatite were synthesized by a hydroxyapatite particles kneading method. The preparation method, characterization, and the results of corneal cell adhesion and proliferation on the composite material were studied. PVA-COL-HAp composites were successfully synthesized. A micro-porous structure of the PVA-COL-HAp could be introduced by hydrochloric acid treatment and the porosity could be controlled by the pH of the hydrochloric acid solution, the treatment time, and the crystallinity of the HAp particles. Chick embryonic keratocyto-like cells were well attached and proliferated on the PVA-COL-HAp composites. This material showed potential for keratoprosthesis application. Further study such as a long-term animal study is now required

Synthesis and characterization of hydroxyapatite-gelatine composite materials for orthopaedic application

Energy Technology Data Exchange (ETDEWEB)

Yanovska, A., E-mail: biophy@yandex.ru [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Kuznetsov, V. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Stanislavov, A. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Husak, E. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine); Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Pogorielov, M. [Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Starikov, V. [National Technical University ”Kharkov Polytechnic Institute”, 21 Frunze Str., 61002, Kharkov (Ukraine); Bolshanina, S. [Sumy State University, Ministry of Education and Science of Ukraine, 2 R. Korsakova Str., 40007, Sumy (Ukraine); Danilchenko, S. [Institute of Applied Physics, National Academy of Sciences of Ukraine, 58 Petropavlovskaya Str., 40000, Sumy (Ukraine)

2016-11-01

The composite materials based on hydroxyapatite (HA) and gelatine (Gel) with addition of silver and zirconium oxide were obtained. The study investigates a combination of low powered ultrasonic irradiation and low concentration of gelatine in the co-precipitation synthesis. These composites have different weight ratios of organic/inorganic components and may be synthesized in two ways: simple mixing and co-precipitation. Both of which were compared. The estimation of porosity, in vivo testing, surface morphology and phase composition as well as the IR-analysis were provided. Hydroxyapatite was the main crystalline phase in obtained composites. While around powdered HA-Gel composite the connective tissue capsule is formed without bone tissue formation, HA-Gel-Ag porous composite implantation leads to formation of new bone tissue and activation of cell proliferation. Addition of silver ions into composite material allows decreasing inflammation on the first stage of implantation and has positive effect on bone tissue formation. Some of the obtained composite materials containing silver or ZrO{sub 2} are biocompatible. bio-resorbable and osteoconductive with high level of porosity (75–85%). - Highlights: • Hydroxyapatite-gelatine composites with addition of Ag{sup +} and ZrO{sub 2} were obtained. • Composites were synthesized in two ways: simple mixing and co-precipitation. • Co-precipitation synthesis combined ultrasonic treatment and low concentration of gelatine. • Obtained composites have different weight ratios of organic/inorganic components. • Some composites are osteoconductive and all of them have high level of porosity (75–85%).

Characterization of x-ray diffraction and electron spin resonance: Effects of sintering time and temperature on bovine hydroxyapatite

International Nuclear Information System (INIS)

Kusrini, Eny; Sontang, Muhammad

2012-01-01

The physical and chemical properties of a hydroxyapatite produced by the sintering of bovine bone were investigated by powder x-ray diffraction (PXRD), electron spin resonance (ESR), energy dispersive x-ray spectroscopy (EDX), scanning electron microscopy (SEM), Fourier transform infrared (FTIR), and differential thermal analysis (DTA). A bovine bone powder was sintered at different temperatures ranging from 500 to 1400 °C. The influences of post-irradiation storage on the radiation ESR response of the bovine bone powder before and after sintering were also studied. The results indicate that the sintered bovine bone powder contained hydroxyapatite. Diffraction patterns were sharp and clear based on the (211), (300), and (202) reflections corresponding to bovine hydroxyapatite (BHA), which confirmed the phase purity and high crystalline grade of the BHA produced. The PXRD profile of BHA was dependent on sintering temperatures and times. The molecular formula of BHA was determined by Rietveld analysis showed a similar structure and composition to calcium hydroxyapatite in hexagonal P6 3 /m space group a=b=9.435 Å and c=6.895 Å. ESR data showed that the sintering process can decrease the number of free radicals in BHA; it also revealed that the number of free radicals is constant during long storage periods (75 days). The sintering technique described in this study may be used to extract hydroxyapatite from biowaste bovine bone, leading to its application as a bone filler. - Highlights: ► Natural hydroxyapatite was produced from the bio-wasting bovine bones by sintering method. ► PXRD profile of BHA is dependent on the different temperatures and times in sintering process. ► ESR data is useful to study the typical of free radicals formed in the samples after irradiation. ► Stability and physicochemical properties of BHA is dependent on the different storage times. ► Technique is able to be used to find the natural hydroxyapatite applicable for bone filler.

Influence of fluorine substitution on the morphology and structure of hydroxyapatite nanocrystals prepared by hydrothermal method

International Nuclear Information System (INIS)

Joseph Nathanael, A.; Mangalaraj, D.; Hong, S.I.; Masuda, Y.; Rhee, Y.H.; Kim, H.W.

2013-01-01

Hydroxyapatite (HAp) nanocrystals with different levels of fluorine substitution (P/F = 0, 6, 4 and 2) on the OH sites were produced via hydrothermal method. The fluorine substitution was found to alter the morphology of crystals appreciably. The aspect ratio and the crystallinity of HAp crystals increased with increasing fluorine substitution. The presence of broad ring and hallow ring patterns in electron diffraction suggests the low-crystalline nature of HAp crystals. With increasing fluorine substitution, the diffraction patterns exhibited discrete rings and numerous diffraction spots, implying the increased crystallinity. Raman spectra from the HAp nanoparticles also support the less-crystalline nature of the pristine HAp and the enhanced crystallization by fluorine substitution. In HAp crystals processed with no fluorine substitution, surface energy and planar Ca 2+ density are less sensitive to the crystallographic orientation because of its low-crystalline nature, favoring equi-axed or slightly elongated particles. The addition of fluorine apparently increased the crystallinity, enhancing the orientation dependent growth and accordingly the aspect ratio. Osteoblast proliferation was observed to be enhanced by fluorine substitution in HAp. In vitro biological data support that the excellent osteoblastic cell viability and functional activity of the fluoridated apatite. -- Highlights: ► Fluorapatite nanorods were produced hydrothermally with different fluorine content. ► Fluorine substitution was found to alter the morphology of crystals appreciably. ► It enhances the crystallinity, orientation dependent growth and hence aspect ratio. ► In vitro cellular analysis shows excellent cell viability of the fluorapatite.

Synthesis of Biocompatible Nanoparticulate Coordination Polymers for Diagnostic and Therapeutic Applications

Science.gov (United States)

Kandanapitiye, Murthi S.

The combination of nanotechnology with medicinal chemistry has developed into a burgeoning research area. Nanomaterials (NMs) could be seamlessly interfaced with various facets in biology, biochemistry, medicinal chemistry and environmental chemistry that may not be available to the same material in the bulk scale. This dissertation research has focused on the development of nanoparticulate coordination polymers for diagnostic and therapeutic applications. Modern imaging techniques include X-ray computed tomography (CT), magnetic resonance imaging (MRI), single photon emission computed tomography (SPECT) and positron emission tomography (PET). We have successfully developed several types of nanoparticulate diagnostics and therapeutics that have some potential usefulness in biomedicine. Synthesis and characterization of nanoparticulate based PET (Positron emission tomography)/SPECT (Single photon emission computed tomography) are discussed in chapter 3. In chapter 4, preparation and potential utility of non-gadolinium based MRI contrast agent are reported for T1-weighted application. As far as the solely effectiveness of relaxation is concerned, Gd-based T 1-weighted MRI contrast agents have excellent enhancement of image contrast but they have risks of biological toxicity. Consequently, the search for T 1-weighted CAs with high efficacy and low toxicity has gained attention toward the Mn(II) and Fe(III). Fe(III) is considered to be more toxic to cells because free ferric or ferrous ions can catalyze the production of reactive oxygen species via the Fenton reactions. Paramagnetic chelates of Mn(II) could be employed as T1-weighted CAs. However, it is challenging to design and synthesize highly stable Mn(II) complexes that could maintain the integrity when administered to living system. Chapter 4 describes the synthesis and utility of nanoparticulate Mn analogue of Prussian blue (K2Mn 3[FeII(CN)6]2) as an effective T1 MRI contrast agent for cellular imaging X

Submicron and Nanoparticulate Matter Removal by HEPA-Rated Media Filters and Packed Beds of Granular Materials

Science.gov (United States)

Perry, J. L.; Agui, J. H.; Vijayakimar, R

2016-01-01

Contaminants generated aboard crewed spacecraft by diverse sources consist of both gaseous chemical contaminants and particulate matter. Both HEPA media filters and packed beds of granular material, such as activated carbon, which are both commonly employed for cabin atmosphere purification purposes have efficacy for removing nanoparticulate contaminants from the cabin atmosphere. The phenomena associated with particulate matter removal by HEPA media filters and packed beds of granular material are reviewed relative to their efficacy for removing fine (less than 2.5 micrometers) and ultrafine (less than 0.01 micrometers) sized particulate matter. Considerations are discussed for using these methods in an appropriate configuration to provide the most effective performance for a broad range of particle sizes including nanoparticulates.

Hydroxyapatite synthesis using EDTA

Science.gov (United States)

Kang, Nak Heon; Kim, Soon Je; Song, Seung Han; Choi, Sang mun; Choi, Sik Young; Kim, Youn Jung

2013-01-01

Bone comprises structure of body and is consisted of inorganic substances. It exists in an organic structure in the body. Even though it is firm and has self healing mechanism, it can be damaged by trauma, cancer, or bone diseases. Allograft can be an alternative solution for autologous bone graft. Hydroxyapatite(Ca10(PO4)6(OH)2), an excellent candidate for allograft, can be applied to bone defect area. There are several methods to produce hydroxyapatite, however economical cost and time consuming make the production difficult. In this study we synthesized the hydroxyapatite with Ethyenediamine tetraacetic acid. Freeze Dried Bone Allograft(Hans Biomed) was used to be a control group. Synthesized hydroxyapatite was a rod shape, white powdery type substance with 2 ~ 5 μm length and 0.5 ~ 1 μm width. X-ray diffraction showed the highest sharp peak at 32° and high peaks at 25.8°, 39.8°, 46.8°, 49.5°, and 64.0° indicating a similar substance to the freeze Dried Bone Allograft. 3 days after the cell growth of synthesized hydroxyapatite showed 1.5 fold more than the Bone Allograft. Cellular and media alkaline phosphate activity increased similar to the bone alloagraft. In this study we came up with a new method to produce the hydroxyapatite. It is a convenient method that can be held in room temperature and low pressure. Also the the product can be manufactured in large quantity. It can be also transformed into scaffold structure which will perform a stronger configuration. The manufacturing method will help the bony defect patients and make future medical products. PMID:23714942

Hydroxyapatite synthesis using EDTA.

Science.gov (United States)

Kang, Nak Heon; Kim, Soon Je; Song, Seung Han; Choi, Sang mun; Choi, Sik Young; Kim, Youn Jung

2013-05-01

Bone comprises structure of the body and consisted of inorganic substances. It exists in an organic structure in the body. Even though it is firm and has self-healing mechanism, it can be damaged by trauma, cancer, or bone diseases. Allograft can be an alternative solution for autologous bone graft. Hydroxyapatite (Ca10(PO4)6(OH)2), an excellent candidate for allograft, can be applied to bone defect area. There are several methods to produce hydroxyapatite; however, economical cost and being time consuming make the production difficult. In this study, we synthesized hydroxyapatite with EDTA. Freeze-dried bone allograft (Hans Biomed) was used as the control group. Synthesized hydroxyapatite was a rod-shaped, white powdery substance with 2- to 5-μm length and 0.5- to 1-μm width. X-ray diffraction showed the highest sharp peak at 32°C and high peaks at 25.8°C, 39.8°C, 46.8°C, 49.5°C, and 64.0°C, indicating a similar substance to the freeze-dried bone allograft. After 3 days, the cell growth of synthesized hydroxyapatite showed 1.5-fold more than did the bone allograft. Cellular and media alkaline phosphate activity increased similar to the bone allograft. In this study, we came up with a new method to produce the hydroxyapatite. It is a convenient method that can be held in room temperature and low pressure. Also, the product can be manufactured in large quantity. It can be also transformed into scaffold structure, which will perform a stronger configuration. The manufacturing method will help the bony defect patients and make future medical products.

Ellipsometric analysis and optical absorption characterization of gallium phosphide nanoparticulate thin film

International Nuclear Information System (INIS)

Zhang Qi-Xian; Ruan Fang-Ping; Wei Wen-Sheng

2011-01-01

Gallium phosphide (GaP) nanoparticulate thin films were easily fabricated by colloidal suspension deposition via GaP nanoparticles dispersed in N,N-dimethylformamide. The microstructure of the film was performed by x-ray diffraction, high resolution transmission electron microscopy and field emission scanning electron microscopy. The film was further investigated by spectroscopic ellipsometry. After the model GaP+void|SiO 2 was built and an effective medium approximation was adopted, the values of the refractive index n and the extinction coefficient k were calculated for the energy range of 0.75 eV–4.0 eV using the dispersion formula in DeltaPsi2 software. The absorption coefficient of the film was calculated from its k and its energy gaps were further estimated according to the Tauc equation, which were further verified by its fluorescence spectrum measurement. The structure and optical absorption properties of the nanoparticulate films are promising for their potential applications in hybrid solar cells. (condensed matter: electronic structure, electrical, magnetic, and optical properties)

Dynamic mechanical properties of hydroxyapatite/polyethylene oxide nanocomposites: characterizing isotropic and post-processing microstructures

Science.gov (United States)

Shofner, Meisha; Lee, Ji Hoon

2012-02-01

Compatible component interfaces in polymer nanocomposites can be used to facilitate a dispersed morphology and improved physical properties as has been shown extensively in experimental results concerning amorphous matrix nanocomposites. In this research, a block copolymer compatibilized interface is employed in a semi-crystalline matrix to prevent large scale nanoparticle clustering and enable microstructure construction with post-processing drawing. The specific materials used are hydroxyapatite nanoparticles coated with a polyethylene oxide-b-polymethacrylic acid block copolymer and a polyethylene oxide matrix. Two particle shapes are used: spherical and needle-shaped. Characterization of the dynamic mechanical properties indicated that the two nanoparticle systems provided similar levels of reinforcement to the matrix. For the needle-shaped nanoparticles, the post-processing step increased matrix crystallinity and changed the thermomechanical reinforcement trends. These results will be used to further refine the post-processing parameters to achieve a nanocomposite microstructure with triangulated arrays of nanoparticles.

Production of hydroxyapatite from waste mussel shells

Energy Technology Data Exchange (ETDEWEB)

Jones, Mark I; Barakat, Haneen; Patterson, Darrell Alec, E-mail: mark.jones@auckland.ac.nz [Department Chemical and Materials Engineering, University of Auckland, New Zealand Private Bag 92019, Auckland Mail Centre, Auckland, 1142 (New Zealand)

2011-10-29

This work describes the formation of Hydroxyaptite, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, from waste mussel shells from the New Zealand aquaculture industry. The raw shells are first calcined to produce lime (CaO) and then reacted in a purpose built reactor to form the Hydroxyapatite (HA) in a low temperature batch process. The calcination was studied in terms of the effects of temperature, heating rate, holding time, nitrogen flow rate and particle size. The crystals formed in the batch reactor were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS) and X-Ray Photoelectron Spectroscopy (XPS). Optimised conditions in the calcination stage resulted in powder with around 95% conversion to lime. The as-produced HA showed poor crystallinity and the presence of impurities, although both of these features were improved by a suitable post heat treatment process. The post treated material showed good crystallinity and was comparable to commercially produced material. Preliminary biocompatibility experiments showed that the HA stimulated cell growth and promoted mineralization. The production of HA from mussel shells in a room temperature, ambient pressure process is not only a sustainable use of waste material, but also from an industrial point of view the process has considerable potential for reducing costs associated with both starting materials and energy.

Hydroxyapatite coatings for biomedical applications

CERN Document Server

Zhang, Sam

2013-01-01

Hydroxyapatite coatings are of great importance in the biological and biomedical coatings fields, especially in the current era of nanotechnology and bioapplications. With a bonelike structure that promotes osseointegration, hydroxyapatite coating can be applied to otherwise bioinactive implants to make their surface bioactive, thus achieving faster healing and recovery. In addition to applications in orthopedic and dental implants, this coating can also be used in drug delivery. Hydroxyapatite Coatings for Biomedical Applications explores developments in the processing and property characteri

Synthesis and characterization of nano hydroxyapatite using reverse micro emulsions as nano reactors

International Nuclear Information System (INIS)

Amin, S.; Siddique, T.

2015-01-01

In the present work reverse micro emulsion has been employed as nano reactors to synthesize nano crystalline Hydroxyapatite (HA). Two precursors; calcium and phosphate with different counter ions of each were used for the synthesis of HA at two different temperatures. To maintain the emulsified nano reactor, cyclohexane, TX-100 and 1-butanol including phosphate precursor was the continuous phase while aqueous Ca precursor solution was taken as the dispersed phase. Nano crystalline particles thus produced were evaluated on the basis of synthesis route, counter ions and temperature. It has been shown that emulsified nano reactors control the morphology, particle size and minimize phase transformation of HA. Characterizations of nano powder of HA are carried out using x-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), and scanning electron microscopy (SEM). HA crystallite size was found to be in the range of 20-25 nm whereas the morphology of nano particles changed from spheres to rods. (author)

Influence of Growth Parameters on the Formation of Hydroxyapatite (HAp Nanostructures and Their Cell Viability Studies

Directory of Open Access Journals (Sweden)

Murugesan Manoj

2015-02-01

Full Text Available Morphology controlled hydroxyapatite (HAp nanostructures play a vital role in biomedical engineering, tissue regenerative medicine, biosensors, chemotherapeutic applications, environmental remediation, etc. The present work investigates the influence of temperature, pH and time on the growth of HAp nanostructures using a simple, cost effective and surfactant free chemical approach. The obtained HAp nanostructures were systematically investigated by analytical techniques such as XRD, FESEM, EDX, FTIR and Raman spectroscopy. The XRD analysis showed that the hexagonal structure of the hydroxyapatite and average crystallite size was estimated from this analysis. The electron microscopic analysis confirmed the different morphologies obtained by varying the synthesis parameters such as temperature, pH and time. The elemental composition was determined through EDS analysis. FTIR and Raman spectroscopic analysis confirmed the presence of functional groups and the purity and crystallinity of the samples. The biocompatibility and adhesion nature of samples was examined with mouse preosteoblast cells. The obtained results demonstrated good biocompatibility and excellent focal adhesion.

Nanoparticulate cerium dioxide and cerium dioxide-titanium dioxide composite thin films on glass by aerosol assisted chemical vapour deposition

International Nuclear Information System (INIS)

Qureshi, Uzma; Dunnill, Charles W.; Parkin, Ivan P.

2009-01-01

Two series of composite thin films were deposited on glass by aerosol assisted chemical vapour deposition (AACVD)-nanoparticulate cerium dioxide and nanoparticulate cerium dioxide embedded in a titanium dioxide matrix. The films were analysed by a range of techniques including UV-visible absorption spectroscopy, X-ray diffraction, scanning electron microscopy and energy dispersive analysis by X-rays. The AACVD prepared films showed the functional properties of photocatalysis and super-hydrophilicity. The CeO 2 nanoparticle thin films displaying photocatalysis and photo-induced hydrophilicity almost comparable to that of anatase titania.

Nanostructured Si-substituted hydroxyapatite coatings for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Rau, Julietta V., E-mail: giulietta.rau@ism.cnr.it [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Fosca, Marco [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Cacciotti, Ilaria [Università di Roma “Tor Vergata”, Dipartimento di Ingegneria Industriale,UR INSTM “Roma Tor Vergata”, Via del Politecnico, 1-00133 Rome (Italy); Laureti, Sara [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via Salaria km 29.300-00016 Monterotondo Scalo (RM) (Italy); Bianco, Alessandra [Università di Roma “Tor Vergata”, Dipartimento di Ingegneria Industriale,UR INSTM “Roma Tor Vergata”, Via del Politecnico, 1-00133 Rome (Italy); Teghil, Roberto [Università della Basilicata, Dipartimento di Scienze, Via dell' Ateneo Lucano 10-85100, Potenza (Italy)

2013-09-30

In the present work, the Si-HAp coatings were deposited on titanium substrates by Pulsed Laser Deposition technique. For deposition, the Si-HAp targets (1.4 wt.% of Si), produced starting from wet synthesized powders, were used. The properties of coatings were investigated by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, atomic force microscopy and Vickers microhardness. The obtained Si-HAp coatings presented a nanosized structure, proper thickness and hardness for applications in orthopedical and dental surgery, aimed at improving the stability and the osteointegration of bone implants. - Highlights: ► Pulsed Laser Deposition method was applied to coat heated Titanium supports. ► Films were deposited using a target of Silicon-Hydroxyapatite sintered ceramics. ► Nanostructured crystalline hard film was grown replicating target composition. ► Prepared coating could be used for orthopedic and dental implants applications.

Nanostructured Si-substituted hydroxyapatite coatings for biomedical applications

International Nuclear Information System (INIS)

Rau, Julietta V.; Fosca, Marco; Cacciotti, Ilaria; Laureti, Sara; Bianco, Alessandra; Teghil, Roberto

2013-01-01

In the present work, the Si-HAp coatings were deposited on titanium substrates by Pulsed Laser Deposition technique. For deposition, the Si-HAp targets (1.4 wt.% of Si), produced starting from wet synthesized powders, were used. The properties of coatings were investigated by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, atomic force microscopy and Vickers microhardness. The obtained Si-HAp coatings presented a nanosized structure, proper thickness and hardness for applications in orthopedical and dental surgery, aimed at improving the stability and the osteointegration of bone implants. - Highlights: ► Pulsed Laser Deposition method was applied to coat heated Titanium supports. ► Films were deposited using a target of Silicon-Hydroxyapatite sintered ceramics. ► Nanostructured crystalline hard film was grown replicating target composition. ► Prepared coating could be used for orthopedic and dental implants applications

Tantalum-doped hydroxyapatite thin films: Synthesis and characterization

International Nuclear Information System (INIS)

Ligot, S.; Godfroid, T.; Music, D.; Bousser, E.; Schneider, J.M.; Snyders, R.

2012-01-01

To achieve a good bioactivity, magnetron-sputtered (MS) hydroxyapatite (HA) coatings have to be stoichiometric and crystalline. It has also been suggested that doping HA with metallic elements improves its bioactivity but frequently reduces its Young’s modulus. Therefore, efforts are still necessary to identify adequate growth conditions, good doping elements and finally to grow doped HA films. In a first attempt, HA films have been synthesized by MS. Our conditions enabled us to grow at ∼10 nm min −1 stoichiometric and crystallized HA coatings that presented a strong texture. The latter is discussed in view of the competitive growth of the material under the strong electron and ion bombardments used here. Based on ab initio calculations identifying Ta as a promising doping element, we then investigated the growth of Ta-doped hydroxyapatite (HA:Ta) by magnetron co-sputtering. The HA:Ta films were in situ crystallized. Our data reveals that for Ta contents <4.5 at.%, Ta could substitute Ca in the HA cell. For higher doping contents, a deviation from the stoichiometric compound is observed and CaO appears. By nanoindentation, we have measured an elastic modulus of 120 ± 9 GPa for a Ta content of 3 at.%. This value is very close to the value of 110 GPa calculated by ab initio calculations, supporting the substitution scenario. The elasticity drop may be understood by screening of the ionic interaction between constituents in HA upon Ta incorporation.

Preparation and characterization of gelatin–hydroxyapatite composite microspheres for hard tissue repair

Energy Technology Data Exchange (ETDEWEB)

Chao, Shao Ching [Department of Materials Science and Engineering, National Chung Hsing University, 250 Kuo-Kuang Road, Taichung 40227, Taiwan (China); Department of Minimally Invasive Skull Neurosurgery, Neurological Institute, Taichung Veterans General Hospital, 1650 Taiwan Boulevard, Sect. 4, Taichung, Taiwan (China); Department of Neurosurgery, ChangHua Hospital, Ministry of Health and Welfare, 80 Chung Cheng Road, Sect. 2 Chiu Kuan Village, Changhua 500, Taiwan (China); Wang, Ming-Jia; Pai, Nai-Su [Department of Materials Science and Engineering, National Chung Hsing University, 250 Kuo-Kuang Road, Taichung 40227, Taiwan (China); Yen, Shiow-Kang, E-mail: skyen@dragon.nchu.edu.tw [Department of Materials Science and Engineering, National Chung Hsing University, 250 Kuo-Kuang Road, Taichung 40227, Taiwan (China)

2015-12-01

Gelatin–hydroxyapatite composite microspheres composed of 21% gelatin (G) and 79% hydroxyapatite (HA) with uniform morphology and controllable size were synthesized from a mixed solution of Ca(NO{sub 3}){sub 2}, NH{sub 4}H{sub 2}PO{sub 4} and gelatin by a wet-chemical method. Material analyses such as X-ray diffraction (XRD), scanning/transmission electron microscopy examination (SEM/TEM) and inductively coupled plasma-mass spectroscopy (ICP-MS) were used to characterize G–HA microspheres by analyzing their crystalline phase, microstructure, morphology and composition. HA crystals precipitate along G fibers to form nano-rods with diameters of 6–10 nm and tangle into porous microspheres after blending. The cell culture indicates that G–HA composite microspheres without any toxicity could enhance the proliferation and differentiation of osteoblast-like cells. In a rat calvarial defect model, G–HA bioactive scaffolds were compared with fibrin glue (F) and Osteoset® Bone Graft Substitute (OS) for their capacity of regenerating bone. Four weeks post-implantation, new bone, mineralization, and expanded blood vessel area were found in G–HA scaffolds, indicating greater osteoconductivity and bioactivity than F and OS. - Highlights: • G–HA composite microspheres were prepared by hydroxyapatite and gelatin. • In vitro tests indicated that the G–HA microspheres were biocompatible and bioactive. • In in vitro tests, G–HA microspheres could be applied in hard tissue engineering. • G–HA had healed the bone defect and provides a high proportion of surface area to open space.

Effect of Zn2+, Fe3+ and Cr3+ addition to hydroxyapatite for its application as an active constituent of sunscreens

Science.gov (United States)

de Araujo, T. S.; de Souza, S. O.; de Sousa, E. M. B.

2010-11-01

Biocompatible phosphate materials are used in different applications like bone and dental implants, drug delivery systems and others, but could also be applied in inorganic sunscreens. Using sunscreens is extremely necessary, because long time exposure to sun can cause skin cancer. In this work chemical precipitation method has been used to produce hydroxyapatite. Cr3+, Zn2+ and Fe3+ doped samples were characterized using powder X-Ray Diffraction (XRD) and Optical Absorption techniques. X-ray diffraction measurements confirmed the materials were in the expected crystalline structures. The crystallite size as measured from the X-ray pattern was 23-27 nm (±1). The absorption spectra in the ultraviolet and visible ranges indicate that appropriately doped and sized hydroxyapatite particles may have potential applications as active constituents of sunscreens.

Crystallization of modified hydroxyapatite on titanium implants

International Nuclear Information System (INIS)

Golovanova, O A; Izmailov, R R; Zaits, A V; Ghyngazov, S A

2016-01-01

Carbonated-hydroxyapatite (CHA) and Si-hydroxyapatite (Si-HA) precipitation have been synthesized from the model bioliquid solutions (synovial fluid and SBF). It is found that all the samples synthesized from the model solutions are single-phase and represent hydroxyapatite. The crystallization of the modified hydroxyapatite on alloys of different composition, roughness and subjected to different treatment techniques was investigated. Irradiation of the titanium substrates with the deposited biomimetic coating can facilitate further growth of the crystal and regeneration of the surface. (paper)

Influence of fluorine substitution on the morphology and structure of hydroxyapatite nanocrystals prepared by hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Joseph Nathanael, A., E-mail: ajosephnc@yahoo.com [Department of Nanomaterials Engineering, Chungnam National University, Daejeon 305-764 (Korea, Republic of); Thin Film and Nanomaterials Laboratory, Department of Physics, Bharathiar University, Coimbatore 641 046 (India); Mangalaraj, D., E-mail: dmraj800@yahoo.com [Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641 046 (India); Hong, S.I., E-mail: sihong@cnu.ac.kr [Thin Film and Nanomaterials Laboratory, Department of Physics, Bharathiar University, Coimbatore 641 046 (India); Masuda, Y. [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya 463-8560 (Japan); Rhee, Y.H.; Kim, H.W. [Department of Microbiology, Chungnam National University, Daejeon 305-764 (Korea, Republic of)

2013-01-15

Hydroxyapatite (HAp) nanocrystals with different levels of fluorine substitution (P/F = 0, 6, 4 and 2) on the OH sites were produced via hydrothermal method. The fluorine substitution was found to alter the morphology of crystals appreciably. The aspect ratio and the crystallinity of HAp crystals increased with increasing fluorine substitution. The presence of broad ring and hallow ring patterns in electron diffraction suggests the low-crystalline nature of HAp crystals. With increasing fluorine substitution, the diffraction patterns exhibited discrete rings and numerous diffraction spots, implying the increased crystallinity. Raman spectra from the HAp nanoparticles also support the less-crystalline nature of the pristine HAp and the enhanced crystallization by fluorine substitution. In HAp crystals processed with no fluorine substitution, surface energy and planar Ca{sup 2+} density are less sensitive to the crystallographic orientation because of its low-crystalline nature, favoring equi-axed or slightly elongated particles. The addition of fluorine apparently increased the crystallinity, enhancing the orientation dependent growth and accordingly the aspect ratio. Osteoblast proliferation was observed to be enhanced by fluorine substitution in HAp. In vitro biological data support that the excellent osteoblastic cell viability and functional activity of the fluoridated apatite. -- Highlights: Black-Right-Pointing-Pointer Fluorapatite nanorods were produced hydrothermally with different fluorine content. Black-Right-Pointing-Pointer Fluorine substitution was found to alter the morphology of crystals appreciably. Black-Right-Pointing-Pointer It enhances the crystallinity, orientation dependent growth and hence aspect ratio. Black-Right-Pointing-Pointer In vitro cellular analysis shows excellent cell viability of the fluorapatite.

Investigating the addition of SiO₂-CaO-ZnO-Na₂O-TiO₂ bioactive glass to hydroxyapatite: Characterization, mechanical properties and bioactivity.

Science.gov (United States)

Yatongchai, Chokchai; Placek, Lana M; Curran, Declan J; Towler, Mark R; Wren, Anthony W

2015-11-01

Hydroxyapatite (Ca10(PO4)6(OH)2) is widely investigated as an implantable material for hard tissue restoration due to its osteoconductive properties. However, hydroxyapatite in bulk form is limited as its mechanical properties are insufficient for load-bearing orthopedic applications. Attempts have been made to improve the mechanical properties of hydroxyapatite, by incorporating ceramic fillers, but the resultant composite materials require high sintering temperatures to facilitate densification, leading to the decomposition of hydroxyapatite into tricalcium phosphate, tetra-calcium phosphate and CaO phases. One method of improving the properties of hydroxyapatite is to incorporate bioactive glass particles as a second phase. These typically have lower softening points which could possibly facilitate sintering at lower temperatures. In this work, a bioactive glass (SiO2-CaO-ZnO-Na2O-TiO2) is incorporated (10, 20 and 30 wt%) into hydroxyapatite as a reinforcing phase. X-ray diffraction confirmed that no additional phases (other than hydroxyapatite) were formed at a sintering temperature of 560 ℃ with up to 30 wt% glass addition. The addition of the glass phase increased the % crystallinity and the relative density of the composites. The biaxial flexural strength increased to 36 MPa with glass addition, and there was no significant change in hardness as a function of maturation. The pH of the incubation media increased to pH 10 or 11 through glass addition, and ion release profiles determined that Si, Na and P were released from the composites. Calcium phosphate precipitation was encouraged in simulated body fluid with the incorporation of the bioactive glass phase, and cell culture testing in MC-3T3 osteoblasts determined that the composite materials did not significantly reduce cell viability. © The Author(s) 2015.

MRI of orbital hydroxyapatite implants

International Nuclear Information System (INIS)

Flanders, A.E.; De Potter P.; Rao, V.M.; Tom, B.M.; Shields, C.L.; Shields, J.A.

1996-01-01

Our aim was to use MRI for the postsurgical assessment of a new form of integrated orbital implant composed of a porous calcium phosphate hydroxyapatite substrate. We studied ten patients 24-74 years of age who underwent enucleation and implantation of a hydroxyapatite ball; 5-13 months after surgery, each patient was examined by spin-echo MRI, with fat suppression and gadolinium enhancement. Fibrovascular ingrowth was demonstrated in all ten patients as areas of enhancement at the periphery of the hydroxyapatite sphere that extended to the center to a variable degree. The radiologist should aware of the MRI appearances of the coralline hydroxyapatite orbital implant since it is now widely used following enucleation. MRI is a useful means to determine successful incorporation of the substrate into the orbital tissues. The normal pattern of contrast enhancement should not be mistaken for recurrent tumor or infection. (orig.)

Facial skeletal augmentation using hydroxyapatite cement.

Science.gov (United States)

Shindo, M L; Costantino, P D; Friedman, C D; Chow, L C

1993-02-01

This study investigates the use of a new calcium phosphate cement, which sets to solid, microporous hydroxyapatite, for facial bone augmentation. In six dogs, the supraorbital ridges were augmented bilaterally with this hydroxyapatite cement. On one side, the hydroxyapatite cement was placed directly onto the bone within a subperiosteal pocket. On the opposite side, the cement was contained within a collagen membrane tubule and then inserted into a subperiosteal pocket. The use of collagen tubules facilitated easy, precise placement of the cement. All implants maintained their original augmented height throughout the duration of the study. They were well tolerated without extrusion or migration, and there was no significant sustained inflammatory response. Histologic studies, performed at 3, 6, and 9 months revealed that when the cement was placed directly onto bone, progressive replacement of the implant by bone (osseointegration of the hydroxyapatite with the underlying bone) without a loss of volume was observed. In contrast, when the cement-collagen tubule combination was inserted, primarily a fibrous union was noted. Despite such fibrous union, the hydroxyapatite-collagen implant solidly bonded to the underlying bone, and no implant resorption was observed. Hydroxyapatite cement can be used successfully for the experimental augmentation of the craniofacial skeleton and may be applicable for such uses in humans.

Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold

International Nuclear Information System (INIS)

Ciobanu, Gabriela; Ilisei, Simona; Luca, Constantin

2014-01-01

The present paper is focused on a study regarding the possibility of obtaining hydroxyapatite-silver nanoparticle coatings on porous polyurethane scaffold. The method applied is based on a combined strategy involving hydroxyapatite biomimetic deposition on polyurethane surface using a Supersaturated Calcification Solution (SCS), combined with silver ions reduction and in-situ crystallization processes on hydroxyapatite-polyurethane surface by sample immersing in AgNO 3 solution. The morphology, composition and phase structure of the prepared samples were characterized by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS) measurements. The data obtained show that a layer of hydroxyapatite was deposited on porous polyurethane support and the silver nanoparticles (average size 34.71 nm) were dispersed among and even on the hydroxyapatite crystals. Hydroxyapatite/polyurethane surface acts as a reducer and a stabilizing agent for silver ions. The surface plasmon resonance peak in UV-Vis absorption spectra showed an absorption maximum at 415 nm, indicating formation of silver nanoparticles. The hydroxyapatite-silver polyurethane scaffolds were tested against Staphylococcus aureus and Escherichia coli and the obtained data were indicative of good antibacterial properties of the materials. - Highlights: • The hydroxyapatite and silver nanoparticles were grown on the polyurethane scaffold • The hydroxyapatite/polyurethane acts as reducing agent, stabilizer and matrix for Ag • The samples were well characterized by SEM-EDX, XRD, XPS, UV-visible spectroscopy • The hydroxyapatite/silver polyurethane scaffold shows antibacterial property

Biocompatible nanocrystalline natural bonelike carbonated hydroxyapatite synthesized by mechanical alloying in a record minimum time

Energy Technology Data Exchange (ETDEWEB)

Lala, S. [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan-713104, West Bengal (India); Brahmachari, S.; Das, P.K. [Department of Biological Chemistry, Indian Association for the Cultivation of Science, Jadavpur, Kolkata-700 032 (India); Das, D. [UGC-DAE Consortium for Scientific Research, Kolkata-700098 (India); Kar, T. [Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata-700032 (India); Pradhan, S.K., E-mail: skp_bu@yahoo.com [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan-713104, West Bengal (India)

2014-09-01

Single phase nanocrystalline biocompatible A-type carbonated hydroxyapatite (A-cHAp) powder has been synthesized by mechanical alloying the stoichiometric mixture of CaCO{sub 3} and CaHPO{sub 4}.2H{sub 2}O powders in open air at room temperature within 2 h of milling. The A-type carbonation in HAp is confirmed by FTIR analysis. Structural and microstructure parameters of as-milled powders are obtained from both Rietveld's powder structure refinement analysis and transmission electron microscopy. Size and lattice strain of nanocrystalline HAp particles are found to be anisotropic in nature. Mechanical alloying causes amorphization of a part of crystalline A-cHAp which is analogous to native bone mineral. Some primary bond lengths of as-milled samples are critically measured. MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assay test reveals high percentage of cell viability and hence confirms the biocompatibility of the sample. The overall results indicate that the processed A-cHAp has a chemical composition very close to that of biological apatite. - Graphical abstract: Biocompatible A-Type Carbonated Hydroxyapatite (A-cHAp) has been synthesized by mechanical alloying in polycrystalline form within 2 h of milling. The shape and position of CO channel have been shown. - Highlights: • A-cHAp phase is completed within 2 h of milling. • FTIR analysis confirms A-type carbonation in HAp. • Amorphization of a part of crystalline A-cHAp. • Particle size and strain are anaisotropic in nature. • High cell viability under MTT assay.

Hydroxyapatite-lignin composite as a metallic implant-bone tissue osseointegration improver: experimental study in dogs

Directory of Open Access Journals (Sweden)

Fabrício Luciani Valente

2015-01-01

Full Text Available The study aimed to evaluate biocompatibility, osteoconduction and osseointegration of a pasty composite of hydroxyapatite (20% and lignin (80% as a promoter of metal implant and bone tissue integration. An intramedullary Schanz pin was implanted in both tibias of fifteen bitches. In the left tibia, the pin was coated with the biomaterial at the time of surgery. Marrow cavity was also filled with the biomaterial. Right limb did not receive the biomaterial, then constituting the control group. Tibias were harvested from five animals at 8, 60 and 150 days after surgery; three of them were analyzed by histological and biomechanical assessment and the two remaining tibias by X-ray diffraction. Results showed that the biomaterial is biocompatible, with osteoconductivity and osseointegration properties. Histological analysis and diffractograms showed the presence of hydroxyapatite in samples in all periods, although the presence of organic material of low crystallinity was variable. There was no statistical difference in the forces required for removal of the biocompatibility, osteoconductivity and osseointegration, it was not able to promote a better intramedullary pin anchorage.

Characterization of dicalcium phosphate dihydrate cements prepared using a novel hydroxyapatite-based formulation

International Nuclear Information System (INIS)

Alge, Daniel L; Cruz, Grace Santa; Chu, Tien-Min Gabriel; Goebel, W Scott

2009-01-01

Dicalcium phosphate dihydrate (DCPD) cements are typically prepared using β-tricalcium phosphate (β-TCP) as the base component. However, hydroxyapatite (HA) is an interesting alternative because of its potential for reducing cement acidity, as well as modulating cement properties via ionic substitutions. In the present study, we have characterized DCPD cements prepared with a novel formulation based on monocalcium phosphate monohydrate (MCPM) and HA. Cements were prepared using a 4:1 MCPM:HA molar ratio. The reactivity of HA in this system was verified by showing DCPD formation using poorly crystalline HA, as well as highly crystalline HA. Evaluation of cements prepared with poorly crystalline HA revealed that setting occurs rapidly in the MCPM/HA system, and that the use of a setting regulator is necessary to maintain workability of the cement paste. Compressive testing showed that MCPM/HA cements have strengths comparable to what has previously been published for DCPD cements. However, preliminary in vitro analysis of cement degradation revealed that conversion of DCPD to HA may occur much more rapidly in the MCPM/HA system compared to cements prepared with β-TCP. Future studies should investigate this property further, as it could have important implications for the use of HA-based DCPD cement formulations.

Strontium substituted hydroxyapatites: Synthesis and determination of their structural properties, in vitro and in vivo performance

Energy Technology Data Exchange (ETDEWEB)

Kaygili, Omer, E-mail: okaygili@firat.edu.tr [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey); Keser, Serhat [Department of Chemistry, Faculty of Science, Firat University, 23119 Elazig (Turkey); Kom, Mustafa [Department of Surgery, Faculty of Veterinary Medicine, Firat University, 23119 Elazig (Turkey); Eroksuz, Yesari [Department of Pathology, Faculty of Veterinary Medicine, Firat University, 23119 Elazig (Turkey); Dorozhkin, Sergey V. [Kudrinskaja square 1-155, Moscow 123242 (Russian Federation); Ates, Tankut [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey); Ozercan, Ibrahim H. [Department of Pathology, School of Medicine, Firat University, 23119 Elazig (Turkey); Tatar, Cengiz; Yakuphanoglu, Fahrettin [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey)

2015-10-01

The objective of this study is to present a detailed report related to the synthesis and characterization of strontium substituted hydroxyapatites. Based on this purpose, hydroxyapatite (HAp) bioceramics with different amounts of strontium (e.g., 0, 0.45, 0.90, 1.35, 1.80 and 2.25 at.%) were prepared using a sol–gel method. The effects of Sr substitution on the structural properties and biocompatibility of the samples were studied by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM) techniques, in vitro and in vivo tests. All the samples composed of the nanoparticles ranging from 21 to 27 nm. The presence of Sr at low levels influenced the crystal size, crystallinity degree, lattice parameters and volume of the unit cell of the HAp. Both in vitro conditions and soaking period in simulated body fluid (SBF) significantly affected these properties. Especially, the (Ca + Sr)/P molar ratio gradually decreases with increasing soaking period in SBF. Animal experiments revealed the bone formation and osseointegration for all samples, and as compared with other groups, more reasonable, were observed for the sample with the lowest Sr content. - Highlights: • Sr content affects the structural properties of hydroxyapatite. • Bone formation and osseointegration are observed for all the samples. • In vitro conditions cause a significant change in the (Ca + Sr)/P ratio.

Synthesis and characterization of new crystalline mesoporous beta-tricalcium phosphate nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Silva, F.R.O.; Yoshito, W.K.; Cosentino, I.C.; Bressiani, A.H.A.; Lima, N.B. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2016-07-01

Full text: Calcium phosphates, including hydroxyapatite [HA, Ca10 (PO4)6(OH)2] and beta-tricalcium phosphate [B-TCP, Ca3(PO4)2], are the main mineral component of bone tissue and teeth. The synthetic calcium phosphates are of special interest in medicine because of their biocompatibility, bioactivity and non-toxicity. B-TCP is advantageous to HA for drug delivery system due to their high solubility and controllable bioresorption rate. To obtain B-TCP, the literature reports the transformation of calcium deficient hydroxyapatite (CDHA) to ?-TCP since it couldnot be synthesized directly in aqueous solution, until now. For the first time, B-TCP have been successfully synthesized by wet precipitation method at room temperature with a Ca/P molar ratio equal to 1.5 and pH at 6. The present work is concerned with the preparation of B-TCP and it characterization through XRD, BET and TEM analysis. The results showed well-characterized peaks of crystalline pure B-TCP (JCPDS 09-0169) for the dried powder, with a high BET surface area of 574 ± 7 (m2/g). The TEM micrographs exhibits mesoporous structure, which is suitable as a drug carrier. (author)

Preferential Alignment of Hydroxyapatite Crystallites in Nanocomposites with Chemically Disintegrated Silk Fibroin

International Nuclear Information System (INIS)

Nemoto, Rei; Wang Li; Ikoma, Toshiyuki; Tanaka, Junzo; Senna, Mamoru

2004-01-01

Hydroxyapatite (HAp) nanocrystals were prepared at room temperature by a coprecipitation method from Ca(OH) 2 and H 3 PO 4 , in the presence of chemically disintegrated silk fibroin (SF). Adsorbed amounts of cations on SF and crystallinity of HAp in the composite were increased by the chemical disintegration of SF higher order structure. Preferential alignment of c-axis of HAp crystallites along the longitudinal direction of ca. 150nm SF fibril was observed. These changes due to disintegration of SF were discussed in terms of the chemical interaction between HAp and SF. The resulted composite with preferential alignment of HAp nanocrystals is a good candidate as a starting material for bone substitutes

Spectral analysis of allogeneic hydroxyapatite powders

Science.gov (United States)

Timchenko, P. E.; Timchenko, E. V.; Pisareva, E. V.; Vlasov, M. Yu; Red'kin, N. A.; Frolov, O. O.

2017-01-01

In this paper we discuss the application of Raman spectroscopy to the in vitro analysis of the hydroxyapatite powder samples produced from different types of animal bone tissue during demineralization process at various acid concentrations and exposure durations. The derivation of the Raman spectrum of hydroxyapatite is attempted by the analysis of the pure powders of its known constituents. Were experimentally found spectral features of hydroxyapatite, based on analysis of the line amplitude at wave numbers 950-965 cm-1 ((PO4)3- (ν1) vibration) and 1065-1075 cm-1 ((CO3)2-(ν1) B-type replacement). Control of physicochemical properties of hydroxyapatite was carried out by Raman spectroscopy. Research results are compared with an infrared Fourier spectroscopy.

Spectral analysis of allogeneic hydroxyapatite powders

International Nuclear Information System (INIS)

Timchenko, P E; Timchenko, E V; Pisareva, E V; Vlasov, M Yu; Red’kin, N A; Frolov, O O

2017-01-01

In this paper we discuss the application of Raman spectroscopy to the in vitro analysis of the hydroxyapatite powder samples produced from different types of animal bone tissue during demineralization process at various acid concentrations and exposure durations. The derivation of the Raman spectrum of hydroxyapatite is attempted by the analysis of the pure powders of its known constituents. Were experimentally found spectral features of hydroxyapatite, based on analysis of the line amplitude at wave numbers 950-965 cm -1 ((PO 4 ) 3- (ν 1 ) vibration) and 1065-1075 cm -1 ((CO 3 ) 2- (ν 1 ) B-type replacement). Control of physicochemical properties of hydroxyapatite was carried out by Raman spectroscopy. Research results are compared with an infrared Fourier spectroscopy. (paper)

Synthesis, characterization, in vitro anti-proliferative and hemolytic activity of hydroxyapatite

Science.gov (United States)

Palanivelu, R.; Ruban Kumar, A.

2014-06-01

Hydroxyapatite (Ca10(PO4)6(OH)2, HAP) nanoparticles are widely used in several biomedical applications due to its compositional similarities to bone mineral, excellent biocompatibility and bioactivity, osteoconductivity. In this present investigation, HAP nanoparticles synthesized by precipitation technique using calcium nitrate and di-ammonium phosphate. The crystalline nature and the functional group analysis are confirmed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Fourier transform Raman spectroscopy (FT-Raman) respectively. The morphological observations are ascertained from field emission electron scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). In vitro anti-proliferative and hemolytic activities are carried out on the synthesized HAP samples and the studies reveals that HAP have mild activity against erythrocytes.

Development of hydroxyapatite/polyvinyl alcohol bionanocomposite for prosthesis implants

Science.gov (United States)

Karthik, V.; Pabi, S. K.; Chowdhury, S. K. Roy

2018-02-01

Hydroxyapatite (Ca10(PO4)6(OH)2) has similar structural and chemical properties of natural bone mineral and hence widely used as a bone replacement substitute. Natural bone consists of hydroxyapatite and collagen. For mimicking the natural, in the present work, a sintered porous hydroxyapatite component has been vacuum impregnated with Polyvinyl alcohol (PVA), which has better properties like biocompatibility, biodegradability and water- solubility. Hydroxyapatite powders have been made into nanosize to reduce the melting point and hence the sintering temperature. In the present investigation high energy ball mill is used to produce nano-hydroxyapatite powders in bulk quantity by optimizing the milling parameters using stainless steel grinding media. Pellets of 10 mm diameter have been produced from nano- hydroxyapatite powders under different uniaxial compaction pressures. The pellets have been sintered to form porous compacts. The vacuum impregnation of sintered pallets with PVA solution of different strength has been done to find the optimum impregnation condition. Microhardness, compressive strength, wear loss and haemocompatibility of hydroxyapatite ceramics have been studied before and after impregnation of PVA. The nano- hydroxyapatite/PVA composites have superior mechanical properties and reduced wear loss than the non-impregnated porous nano-hydroxyapatite ceramics.

Synthesis of hydroxyapatite particles in catanionic mixed surfactants template

International Nuclear Information System (INIS)

Tari, Nesa Esmaeilian; Kashani Motlagh, Mohammad M.; Sohrabi, Beheshteh

2011-01-01

Highlights: ►The mixture of cetyltrimethyl ammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) with different ratio were used as the template for synthesizing HAP particles. ► The overall morphology of the obtained powders at anionic-rich region (SDS:CTAB, 99:1) solution is rod like with high regularity. ► In the presence of cationic rich region (SDS:CTAB, 1:99) the resulted particles was sheet like. ► The resulted HAP nano particles in the presence of SDS were rod like but their morphology was less oriented than anionic-rich region. - Abstract: Different morphologies of nano hydroxyapatite particles, Ca 10 (PO 4 ) 6 (OH) 2 (HAP) are prepared by precipitation method using CaCl 2 and H 3 PO 4 (water phase) and the mixture of cationic surfactant cetyltrimethyl ammonium bromide (CTAB) and anionic one sodium dodecyl sulfate (SDS) as template. The mixture of these surfactants in two regions of cationic-rich and anionic-rich form the various aggregations as template. The results show that by changing the ratio of cationic to anionic surfactant in the mixture the morphology of the nano HAP can be controlled. The nano structure of products is studied by the means of X-ray diffraction (XRD), Fourier transmission infrared spectrometer (FT-IR) and scanning electron microscopy (SEM). With this system we could synthesize nano particles of hydroxyapatite with high crystallinity and least agglomeration.

Synthesis of hydroxyapatite particles in catanionic mixed surfactants template

Energy Technology Data Exchange (ETDEWEB)

Tari, Nesa Esmaeilian [Department of Chemistry, Iran University of Science and Technology, Resalat Square, Hengam Street, Tehran (Iran, Islamic Republic of); Kashani Motlagh, Mohammad M., E-mail: M.Kashani@iust.ac.ir [Department of Chemistry, Iran University of Science and Technology, Resalat Square, Hengam Street, Tehran (Iran, Islamic Republic of); Sohrabi, Beheshteh [Department of Chemistry, Iran University of Science and Technology, Resalat Square, Hengam Street, Tehran (Iran, Islamic Republic of)

2011-12-15

Highlights: Black-Right-Pointing-Pointer The mixture of cetyltrimethyl ammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) with different ratio were used as the template for synthesizing HAP particles. Black-Right-Pointing-Pointer The overall morphology of the obtained powders at anionic-rich region (SDS:CTAB, 99:1) solution is rod like with high regularity. Black-Right-Pointing-Pointer In the presence of cationic rich region (SDS:CTAB, 1:99) the resulted particles was sheet like. Black-Right-Pointing-Pointer The resulted HAP nano particles in the presence of SDS were rod like but their morphology was less oriented than anionic-rich region. - Abstract: Different morphologies of nano hydroxyapatite particles, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2} (HAP) are prepared by precipitation method using CaCl{sub 2} and H{sub 3}PO{sub 4} (water phase) and the mixture of cationic surfactant cetyltrimethyl ammonium bromide (CTAB) and anionic one sodium dodecyl sulfate (SDS) as template. The mixture of these surfactants in two regions of cationic-rich and anionic-rich form the various aggregations as template. The results show that by changing the ratio of cationic to anionic surfactant in the mixture the morphology of the nano HAP can be controlled. The nano structure of products is studied by the means of X-ray diffraction (XRD), Fourier transmission infrared spectrometer (FT-IR) and scanning electron microscopy (SEM). With this system we could synthesize nano particles of hydroxyapatite with high crystallinity and least agglomeration.

The fabrication of well-interconnected polycaprolactone/hydroxyapatite composite scaffolds, enhancing the exposure of hydroxyapatite using the wire-network molding technique.

Science.gov (United States)

Cho, Yong Sang; Hong, Myoung Wha; Jeong, Hoon-Jin; Lee, Seung-Jae; Kim, Young Yul; Cho, Young-Sam

2017-11-01

In this study, the fabrication method was proposed for the well-interconnected polycaprolactone/hydroxyapatite composite scaffold with exposed hydroxyapatite using modified WNM technique. To characterize well-interconnected scaffolds in terms of hydroxyapatite exposure, several assessments were performed as follows: morphology, mechanical property, wettability, calcium ion release, and cell response assessments. The results of these assessments were compared with those of control scaffolds which were fabricated by precision extruding deposition (PED) apparatus. The control PED scaffolds have interconnected pores with nonexposed hydroxyapatite. Consequently, cell attachment of proposed WNM scaffold was improved by increased hydrophilicity and surface roughness of scaffold surface resulting from the exposure of hydroxyapatite particles and fabrication process using powders. Moreover, cell proliferation and differentiation of WNM scaffold were increased, because the exposure of hydroxyapatite particles may enhance cell adhesion and calcium ion release. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 2315-2325, 2017. © 2016 Wiley Periodicals, Inc.

Fabrication and characterization of novel biomimetic PLLA/cellulose/hydroxyapatite nanocomposite for bone repair applications

Energy Technology Data Exchange (ETDEWEB)

Eftekhari, Samin [Department of Chemical Engineering, Ryerson University, 350 Victoria Street, Toronto, ON M5B 2K3 (Canada); El Sawi, Ihab; Bagheri, Zahra Shaghayegh [Department of Mechanical and Industrial Engineering, Ryerson University, 350 Victoria Street, Toronto, ON M5B 2K3 (Canada); Turcotte, Ginette [Department of Chemical Engineering, Ryerson University, 350 Victoria Street, Toronto, ON M5B 2K3 (Canada); Bougherara, Habiba, E-mail: habiba.bougherara@ryerson.ca [Department of Mechanical and Industrial Engineering, Ryerson University, 350 Victoria Street, Toronto, ON M5B 2K3 (Canada)

2014-06-01

The purpose of this research is to develop and characterize a novel biomimetic nanocomposite that closely mimics the properties of real bone such as morphology, composition and mechanical characteristics. This novel porous nanocomposite is composed of cotton-sourced cellulose microcrystals, hydroxyapatite nanoparticles and poly L-lactide acid. A unique combination of commonly used fabrication procedures has been developed including pre-treatment of particles using a coupling agent. The effect of various weight ratios of the reinforcing agents was evaluated to assess their influence on the chemical, thermal, and mechanical properties of the nanocomposites. The prepared nanocomposites were characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, differential scanning calorimetry and compression testing. Our results indicated the presence of molecular interactions between all components leading to an increase of the crystallinity of the polymer from 50% to 80%. Compression test results revealed that increasing the weight ratio of microcrystalline cellulose/poly L-lactide acid and hydroxyapatite/poly L-lactide acid from 0.1 to 0.5 enhanced the compressive yield stress from 0.127 to 2.2 MPa and The Young's modulus from 6.6 to 38 MPa, respectively. It was found that the fabricated nanocomposites are comparable with the trabecular bone from compositional, structural, and mechanical point of view. - Highlights: • Fabrication of PLLA/HA/cellulose composites that mimic the spongeous bone • Homogenous dispersion of the reinforcing agents in the PLLA matrix was attained. • More efficient interface between the PLLA and the reinforcing agents was achieved. • Preliminary in vitro biocompatibility test showed the nontoxicity of the composite. • The crystallinity, the compressive strength and modulus were investigated.

Improved mechanical properties of hydroxyapatite whisker-reinforced poly(L-lactic acid) scaffold by surface modification of hydroxyapatite.

Science.gov (United States)

Fang, Zhou; Feng, Qingling

2014-02-01

To improve the mechanical properties of porous hydroxyapatite/poly(L-lactic acid) (HA/PLLA) composites, HA whiskers with high crystallinity and high aspect ratio were synthesized. HA whiskers were modified with γ-aminopropyltriethoxysilane (APTES) to improve the interface between HA whiskers and PLLA. The composite scaffold consists of a porous PLLA matrix with HA whiskers distributed homogeneously. The morphology and the distributions of pore sizes of PLLA scaffold was not influenced by introducing HA whiskers, while the mechanical properties were improved. Both the compressive strength and compressive modulus were increased with the weight ratio of APTES-modified HA whiskers up to 30 wt.%, but only up to 15 wt.% for non-modified HA whiskers. With more than 15 wt.% HA whiskers, the mechanical properties of HA/PLLA scaffold were better improved with APTES-modified HA whiskers than non-modified. The HA whisker/PLLA scaffold with high porosity and improved mechanical properties is attractive in the application of tissue engineering. Copyright © 2013 Elsevier B.V. All rights reserved.

The distribution of absorptive power dissipation in irradiated nanoparticulate system

International Nuclear Information System (INIS)

Li, Jiayu; Yang, Jian; Gu, Xiaobing

2016-01-01

The knowledge of local radiant absorption is important to the nanostructure optimization, it is beneficial to the applications in energy harvesting, optical heating, photocatalysis, etc. In this paper, FDTD model is constructed for the distribution of absorptive power dissipation in irradiated nanoparticulate system. The theoretical model extended from Mie theory is used to examine the FDTD model, the parameters and conditions set for FDTD simulation are confirmed based on the comparison. Then, the influence of Ag nanoparticle on the absorptive properties of nearby TiO_2 nanoparticle is investigated by FDTD simulation at the wavelength of 0.25 μm. It is indicated that suitable distance between TiO_2 and Ag particles is beneficial to the spectral radiant absorption of TiO_2 particle. Considering the agglomeration of nanoparticles and the oxidation at the TiO_2–Ag interface, the Ag core coated with Al_2O_3 shell is suggested, and the simulated results indicated that the shell thickness and the Ag core size need to be optimized for enhancing the radiant absorption of TiO_2 particle. - Highlights: • The absorptive power distribution in nanoparticulate system is simulated by FDTD. • FDTD simulation is compared with theoretical model extended from Mie theory. • The parameters and conditions are confirmed based on the comparison. • The influence of Ag nanoparticle on nearby TiO_2 particle's absorption is analyzed.

Mediatorless bioelectrocatalysis of dioxygen reduction at indium-doped tin oxide (ITO) and ITO nanoparticulate film electrodes

Energy Technology Data Exchange (ETDEWEB)

Rozniecka, Ewa; Jonsson-Niedziolka, Martin; Sobczak, Janusz W. [Institute of Physical Chemistry, Polish Academy of Sciences, ul. Kasprzaka 44/52, 01-224 Warszawa (Poland); Opallo, Marcin, E-mail: mopallo@ichf.edu.pl [Institute of Physical Chemistry, Polish Academy of Sciences, ul. Kasprzaka 44/52, 01-224 Warszawa (Poland)

2011-10-01

Highlights: > We introduced ITO nanoparticulate films for enzyme immobilization. > The material promotes mediatorless bioelectrocatalysis towards dioxygen reduction. > The electrocatalytical current increase with the thickness of nanoparticulate film. > There is no difference in electrocatalytic current in the presence or absence of mediator. > The stability of the electrode can be improved by crosslinking of the enzyme with bovine serum albumin and glutaraldehyde. - Abstract: Bilirubin oxidase was immobilised on ITO electrodes: bare or covered by ITO nanoparticulate film. The latter material was obtained by immersion and withdrawal of the substrate into ITO nanoparticles suspension. Formation of a protein deposit was confirmed by scanning electron microscopy, atomic force microscopy and X-ray photoelectron spectroscopy. The electrode surface is covered by a protein film in the form of globular aggregates and it exhibits mediatorless electrocatalytic activity towards dioxygen reduction to water at pH 4.8. Modification of the electrode with ITO particles increases its catalytic activity about ten times up to 110 {mu}A cm{sup -2} seen for electrodes prepared by twelve immersion and withdrawal steps into ITO nanoparticle suspension. The catalytic activity is almost unaffected by addition of mediator to solution. The stability of the electrodes is increased by cross-linking of the enzyme with bovine serum albumin and glutaraldehyde. This electrode was applied as biocathode in a zinc-dioxygen battery operating in 0.1 mol dm{sup -3} McIlvaine buffer (pH 4.8).

Mediatorless bioelectrocatalysis of dioxygen reduction at indium-doped tin oxide (ITO) and ITO nanoparticulate film electrodes

International Nuclear Information System (INIS)

Rozniecka, Ewa; Jonsson-Niedziolka, Martin; Sobczak, Janusz W.; Opallo, Marcin

2011-01-01

Highlights: → We introduced ITO nanoparticulate films for enzyme immobilization. → The material promotes mediatorless bioelectrocatalysis towards dioxygen reduction. → The electrocatalytical current increase with the thickness of nanoparticulate film. → There is no difference in electrocatalytic current in the presence or absence of mediator. → The stability of the electrode can be improved by crosslinking of the enzyme with bovine serum albumin and glutaraldehyde. - Abstract: Bilirubin oxidase was immobilised on ITO electrodes: bare or covered by ITO nanoparticulate film. The latter material was obtained by immersion and withdrawal of the substrate into ITO nanoparticles suspension. Formation of a protein deposit was confirmed by scanning electron microscopy, atomic force microscopy and X-ray photoelectron spectroscopy. The electrode surface is covered by a protein film in the form of globular aggregates and it exhibits mediatorless electrocatalytic activity towards dioxygen reduction to water at pH 4.8. Modification of the electrode with ITO particles increases its catalytic activity about ten times up to 110 μA cm -2 seen for electrodes prepared by twelve immersion and withdrawal steps into ITO nanoparticle suspension. The catalytic activity is almost unaffected by addition of mediator to solution. The stability of the electrodes is increased by cross-linking of the enzyme with bovine serum albumin and glutaraldehyde. This electrode was applied as biocathode in a zinc-dioxygen battery operating in 0.1 mol dm -3 McIlvaine buffer (pH 4.8).

Valorization of Bone Waste of Saudi Arabia by Synthesizing Hydroxyapatite.

Science.gov (United States)

Amna, Touseef

2018-05-09

At present, hydroxyapatite is being frequently used for diverse biomedical applications as it possesses excellent biocompatibility, osteoconductivity, and non-immunogenic characteristics. The aim of the present work was to recycle bone waste for synthesis of hydroxyapatite nanoparticles to be used as bone extracellular matrix. For this reason, we for the first time utilized bio-waste of cow bones of Albaha city. The residual bones were utilized for the extraction of natural bone precursor hydroxyapatite. A facile scientific technique has been used to synthesize hydroxyapatite nanoparticles through calcinations of wasted cow bones without further supplementation of chemicals/compounds. The obtained hydroxyapatite powder was ascertained using physicochemical techniques such as XRD, SEM, FTIR, and EDX. These analyses clearly show that hydroxyapatite from native cow bone wastes is biologically and physicochemically comparable to standard hydroxyapatite, commonly used for biomedical functions. The cell viability and proliferation over the prepared hydroxyapatite was confirmed with CCk-8 colorimetric assay. The morphology of the cells growing over the nano-hydroxyapatite shows that natural hydroxyapatite promotes cellular attachment and proliferation. Hence, the as-prepared nano-hydroxyapatite can be considered as cost-effective source of bone precursor hydroxyapatite for bone tissue engineering. Taking into account the projected demand for reliable bone implants, the present research work suggested using environment friendly methods to convert waste of Albaha city into nano-hydroxyapatite scaffolds. Therefore, besides being an initial step towards accomplishment of projected demands of bone implants in Saudi Arabia, our study will also help in reducing the environmental burden by recycling of bone wastes of Albaha city.

Study on carbonated hydroxyapatite as a thermoluminescence dosimeter

International Nuclear Information System (INIS)

Shafaei, M.; Sardari, D.; Ziaie, F.; Larijani, M.M.

2015-01-01

In this study, carbonated hydroxyapatite nanoparticles were used for thermoluminescence dosimetry. The nano-structure carbonated hydroxyapatite synthesized via hydrolysis of CaHPO 4 and CaCO 3 . The obtained nano powders were characterized by XRD technique and FTIR spectroscopy system. The carbonated hydroxyapatite samples were irradiated at different doses using 60 Co gamma rays, and were subjected to thermoluminescence measurement system, consequently. The TL glow curve exhibited two distinguishable peaks centered at around of 165 C and 310 C. The TL response of carbonated hydroxyapatite samples as a function of absorbed dose was linear in the range of 25-1000 Gy. Other dosimetric features of the carbonated hydroxyapatite nanoparticles including fading and reproducibility were also investigated.

Novel hydroxyapatite nanorods improve anti-caries efficacy of enamel infiltrants.

Science.gov (United States)

Andrade Neto, D M; Carvalho, E V; Rodrigues, E A; Feitosa, V P; Sauro, S; Mele, G; Carbone, L; Mazzetto, S E; Rodrigues, L K; Fechine, P B A

2016-06-01

Enamel resin infiltrants are biomaterials able to treat enamel caries at early stages. Nevertheless, they cannot prevent further demineralization of mineral-depleted enamel. Therefore, the aim of this work was to synthesize and incorporate specific hydroxyapatite nanoparticles (HAps) into the resin infiltrant to overcome this issue. HAps were prepared using a hydrothermal method (0h, 2h and 5h). The crystallinity, crystallite size and morphology of the nanoparticles were characterized through XRD, FT-IR and TEM. HAps were then incorporated (10wt%) into a light-curing co-monomer resin blend (control) to create different resin-based enamel infiltrants (HAp-0h, HAp-2h and HAp-5h), whose degree of conversion (DC) was assessed by FT-IR. Enamel caries lesions were first artificially created in extracted human molars and infiltrated using the tested resin infiltrants. Specimens were submitted to pH-cycling to simulate recurrent caries. Knoop microhardness of resin-infiltrated underlying and surrounding enamel was analyzed before and after pH challenge. Whilst HAp-0h resulted amorphous, HAp-2h and HAp-5h presented nanorod morphology and higher crystallinity. Resin infiltration doped with HAp-2h and HAp-5h caused higher enamel resistance against demineralization compared to control HAp-free and HAp-0h infiltration. The inclusion of more crystalline HAp nanorods (HAp-2h and HAp-5h) increased significantly (p<0.05) the DC. Incorporation of more crystalline HAp nanorods into enamel resin infiltrants may be a feasible method to improve the overall performance in the prevention of recurrent demineralization (e.g. caries lesion) in resin-infiltrated enamel. Copyright © 2016 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Synthetic Hydroxyapatite as a Biomimetic Oral Care Agent.

Science.gov (United States)

Enax, Joachim; Epple, Matthias

Human tooth enamel consists mostly of minerals, primarily hydroxyapatite, Ca10(PO4)6(OH)2, and thus synthetic hydroxyapatite can be used as a biomimetic oral care agent. This review describes the synthesis and characterization of hydroxyapatite from a chemist's perspective and provides an overview of its current use in oral care, with a focus on dentin hypersensitivity, caries, biofilm management, erosion, and enamel lesions. Reviews and original research papers published in English and German were included. The efficiency of synthetic hydroxyapatite in occluding open dentin tubules, resulting in a protection for sensitive teeth, has been well documented in a number of clinical studies. The first corresponding studies on caries, biofilm management and erosion have provided evidence for a positive effect of hydroxyapatite either as a main or synergistic agent in oral care products. However, more in situ and in vivo studies are needed due to the complexity of the oral milieu and to further clarify existing results. Due to its biocompatibility and similarity to biologically formed hydroxyapatite in natural tooth enamel, synthetic hydroxyapatite is a promising biomimetic oral care ingredient that may extend the scope of preventive dentistry.

Structural characterization, optical properties and in vitro bioactivity of mesoporous erbium-doped hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Alshemary, Ammar Z.; Akram, Muhammed; Goh, Yi-Fan [Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor Darul Ta’zim (Malaysia); Abdul Kadir, Mohammed Rafiq [Medical Implant Technology Group, Faculty of Biosciences and Medical Engineering, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor Darul Ta’zim (Malaysia); Abdolahi, Ahmad [Faculty of Mechanical Engineering, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor Darul Ta’zim (Malaysia); Hussain, Rafaqat, E-mail: rafaqat@kimia.fs.utm.my [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor Darul Ta’zim (Malaysia)

2015-10-05

Highlights: • Phase pure nano-sized Er doped hydroxyapatite has been prepared. • TEM micrograph confirmed formation of mesoporous material. • Increased Er doping resulted in blue shift with slight increase in energy band gab. • Er-HA showed better dissolution behavior in SBF comparing with pure HA. • Er doping of HA resulted in formation of apatite layer in SBF with Ca/P ratio of 1.72. - Abstract: We report the successful synthesis of mesoporous erbium doped hydroxyapatite (Er-HA, Ca{sub 10−x}Er{sub 2x/3}□{sub x/3}(PO{sub 4}){sub 6}(OH){sub 2}) by using a rapid and efficient microwave assisted wet precipitation method. Characterization techniques like X-ray diffraction (XRD), Fourier transform infra-red (FTIR), X-ray fluorescence spectrometer (XRF), Brunauer, Emmett and Teller (BET) and transmission electron microscopy (TEM) were used to determine lattice parameters, particle size, degree of crystallinity, elemental composition, surface area and morphology of Er-HA. Results confirmed the formation of crystalline Er-HA having crystallite size of 25 nm with spherical and rod like morphology, while the TEM analysis confirmed the mesoporous nature of the particles. Optical spectra of Er-HA contained seven electron transitions, whereas blue shift in the energy band gap (E{sub g}) was observed upon increase in Er{sup 3+} content. The photoluminescence (PL) spectra contained green and red emissions. In vitro bioactivity study conducted in SBF revealed that the incorporation of Er{sup 3+} ions into HA structure lead to the faster discharge of Er{sup 3+} ions resulting in intense growth of apatite grains on the surface of the Er-HA pellets with Ca/P ratio of 1.72.

Design, characterization, and aerosolization of organic solution advanced spray-dried moxifloxacin and ofloxacin dipalmitoylphosphatidylcholine (DPPC) microparticulate/nanoparticulate powders for pulmonary inhalation aerosol delivery

Science.gov (United States)

Duan, Jinghua; Vogt, Frederick G; Li, Xiaojian; Hayes, Don; Mansour, Heidi M

2013-01-01

The aim of this study was to design and develop respirable antibiotics moxifloxacin (MOXI) hydrochloride and ofloxacin (OFLX) microparticles and nanoparticles, and multifunctional antibiotics particles with or without lung surfactant 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) for targeted dry powder inhalation delivery as a pulmonary nanomedicine. Particles were rationally designed and produced by advanced spray-drying particle engineering from an organic solution in closed mode (no water) from dilute solution. Scanning electron microscopy indicated that these particles had both optimal particle morphology and surface morphology, and the particle size distributions were suitable for pulmonary delivery. Comprehensive and systematic physicochemical characterization and in vitro aerosol dispersion performance revealed significant differences between these two fluoroquinolone antibiotics following spray drying as drug aerosols and as cospray-dried antibiotic drug: DPPC aerosols. Fourier transform infrared spectroscopy and confocal Raman microspectroscopy were employed to probe composition and interactions in the solid state. Spray-dried MOXI was rendered noncrystalline (amorphous) following organic solution advanced spray drying. This was in contrast to spray-dried OFLX, which retained partial crystallinity, as did OFLX:DPPC powders at certain compositions. Aerosol dispersion performance was conducted using inertial impaction with a dry powder inhaler device approved for human use. The present study demonstrates that the use of DPPC offers improved aerosol delivery of MOXI as cospray-dried microparticulate/nanoparticulate powders, whereas residual partial crystallinity influenced aerosol dispersion of OFLX and most of the compositions of OFLX:DPPC inhalation powders. PMID:24092972

Mechanical properties and biocompatibility of the sputtered Ti doped hydroxyapatite.

Science.gov (United States)

Vladescu, A; Padmanabhan, S C; Ak Azem, F; Braic, M; Titorencu, I; Birlik, I; Morris, M A; Braic, V

2016-10-01

The hydroxyapatite enriched with Ti were prepared as possible candidates for biomedical applications especially for implantable devices that are in direct contact to the bone. The hydroxyapatites with different Ti content were prepared by RF magnetron sputtering on Ti-6Al-4V alloy using pure hydroxyapatite and TiO2 targets. The content of Ti was modified by changing the RF power fed on TiO2 target. The XPS and FTIR analyses revealed the presence of hydroxyapatite structure. The hardness and elastic modulus of the hydroxyapatite were increased by Ti addition. After 5 days of culture, the cell viability of the Ti-6Al-4V was enhanced by depositing with undoped or doped hydroxyapatite. The Ti additions led to an increase in cell viability of hydroxyapatite, after 5 days of culture. The electron microscopy showed the presence of more cells on the surface of Ti-enriched hydroxyapatite than those observed on the surface of the uncoated alloys or undoped hydroxyapatite. Copyright © 2016 Elsevier Ltd. All rights reserved.

A comparative physico-chemical study of chlorapatite and hydroxyapatite: from powders to plasma sprayed thin coatings.

Science.gov (United States)

Demnati, I; Grossin, D; Combes, C; Parco, M; Braceras, I; Rey, C

2012-10-01

Due to their bioactivity and osteoconductivity, hydroxyapatite (HA) plasma sprayed coatings have been widely developed for orthopedic uses. However, the thermodynamic instability of HA leads frequently to a mixture of phases which limit the functional durability of the coating. This study investigates the plasma spraying of chlorapatite (ClA) powder, known to melt without decomposition, onto pure titanium substrates using a low energy plasma spray system (LEPS). Pure ClA powder was prepared by a solid gas reaction at 950 °C and thermogravimetric analysis showed the good thermal stability of ClA powder in the range 30-1400 °C compared to that of the HA powder. Characterization of ClA coating showed that ClA had a very high crystalline ratio and no other crystalline phase was detected in the coating. HA and ClA coatings composition, microstructure and in vitro bioactivity potential were studied, compared and discussed. In vitro SBF test on HA and ClA coatings revealed the formation of a poorly crystalline apatite on the coating surface suggesting that we could expect a good osteoconductivity especially for the ClA coating prepared by the LEPS system.

The synthesis of hydroxyapatite through the precipitation method.

Science.gov (United States)

Shah, Rizal K; Fahmi, M N; Mat, Akil H; Zainal, Arifin A

2004-05-01

Hydroxyapatite (HA) has been earmarked as suitable for implantation within the human of its chemical makeup to human bone. In this paper, HA powders were synthesized via the precipitation method where phosphoric acid (H3PO4) was titrated into calcium hydroxide solution [Ca(OH)2]. Two parameters such as temperature and stirring rate were identified as factors that influenced the amount and purity of HA powder. Phase identification of the synthesized powder was done using X-Ray Diffraction (XRD). The results show that HA phase can be synthesized from this titration process of Ca(OH)2 and H3PO4 with yield amount of HA powder around 45 - 61 grams but with less than hundred percent purity. In order to study the effect of heat treatment to HA crystals structure, HA powder was calcined at 850 degrees C for 2 hours. It's found that the degree of crystallinity increases after calcination because of lattice expansion when the materials were heated at higher temperature

Osteoconductive hydroxyapatite coated PEEK for spinal fusion surgery

Energy Technology Data Exchange (ETDEWEB)

Hahn, Byung-Dong, E-mail: cera72@kims.re.kr [Functional Ceramics Group, Korea Institute of Materials Science, 797 Changwon-daero, Seongsan-gu, Changwon, Gyeong-Nam, 641-010 (Korea, Republic of); Park, Dong-Soo; Choi, Jong-Jin; Ryu, Jungho; Yoon, Woon-Ha; Choi, Joon-Hwan; Kim, Jong-Woo; Ahn, Cheol-Woo [Functional Ceramics Group, Korea Institute of Materials Science, 797 Changwon-daero, Seongsan-gu, Changwon, Gyeong-Nam, 641-010 (Korea, Republic of); Kim, Hyoun-Ee [School of Materials Science and Engineering, Seoul National University, San 56-1 Sillim-Dong, Gwanak-gu, Seoul, 151-742 (Korea, Republic of); Yoon, Byung-Ho; Jung, In-Kwon [GENOSS, Gyeonggi R and DB Center, Iui-dong, Yeongtong-gu, Suwon, Gyeonggi-do, 443-270 (Korea, Republic of)

2013-10-15

Polyetheretherketone (PEEK) has attracted much interest as biomaterial for interbody fusion cages due to its similar stiffness to bone and good radio-transparency for post-op visualization. Hydroxyapatite (HA) coating stimulates bone growth to the medical implant. The objective of this work is to make an implant consisting of biocompatible PEEK with an osteoconductive HA surface for spinal or orthopedic applications. Highly dense and well-adhered HA coating was developed on medical-grade PEEK using aerosol deposition (AD) without thermal degradation of the PEEK. The HA coating had a dense microstructure with no cracks or pores, and showed good adhesion to PEEK at adhesion strengths above 14.3 MPa. The crystallinity of the HA coating was remarkably enhanced by hydrothermal annealing as post-deposition heat-treatment. In addition, in vitro and in vivo biocompatibility of PEEK, in terms of cell adhesion morphology, cell proliferation, differentiation, and bone-to-implant contact ratio, were remarkably enhanced by the HA coating through AD.

Precipitation of stoichiometric hydroxyapatite by a continuous method

Energy Technology Data Exchange (ETDEWEB)

Gomez-Morales, J.; Boix, T.; Fraile, J.; Rodriguez-Clemente, R. [Consejo Superior de Investigaciones Cientificas, Barcelona (Spain). Inst. de Ciencia de Materiales; Torrent-Burgues, J. [UPC, Barcelona (Spain). Dept. d' Enginyeria Quimica

2001-07-01

In this paper we present the precipitation of hydroxyapatite (HA), Ca{sub 5}(OH)(PO{sub 4}){sub 3}, from highly concentrated CaCl{sub 2} and K{sub 2}HPO{sub 4} solutions, carried out by a continuous method in a MSMPR reactor. The procedure consists of adding the reagents in a ratio Ca to P equal to 1.67, maintaining a temperature of 85 C, inert N{sub 2} atmosphere inside the reactor, and monitoring and adjusting automatically the pH by means of a pH-stat system (pH = 9.0 {+-} 0.1). Under these conditions HA with a Ca to P ratio equal or close to the stoichiometric composition (Ca/P=1.667), with a high yield (up to 99%) and a high production rate (up to 1.17 g/l.min) is obtained at steady state. The CSD, morphology, crystallinity of the precipitates and impurities present fit the requirement for its biomedical applications. (orig.)

Osteoconductive hydroxyapatite coated PEEK for spinal fusion surgery

International Nuclear Information System (INIS)

Hahn, Byung-Dong; Park, Dong-Soo; Choi, Jong-Jin; Ryu, Jungho; Yoon, Woon-Ha; Choi, Joon-Hwan; Kim, Jong-Woo; Ahn, Cheol-Woo; Kim, Hyoun-Ee; Yoon, Byung-Ho; Jung, In-Kwon

2013-01-01

Polyetheretherketone (PEEK) has attracted much interest as biomaterial for interbody fusion cages due to its similar stiffness to bone and good radio-transparency for post-op visualization. Hydroxyapatite (HA) coating stimulates bone growth to the medical implant. The objective of this work is to make an implant consisting of biocompatible PEEK with an osteoconductive HA surface for spinal or orthopedic applications. Highly dense and well-adhered HA coating was developed on medical-grade PEEK using aerosol deposition (AD) without thermal degradation of the PEEK. The HA coating had a dense microstructure with no cracks or pores, and showed good adhesion to PEEK at adhesion strengths above 14.3 MPa. The crystallinity of the HA coating was remarkably enhanced by hydrothermal annealing as post-deposition heat-treatment. In addition, in vitro and in vivo biocompatibility of PEEK, in terms of cell adhesion morphology, cell proliferation, differentiation, and bone-to-implant contact ratio, were remarkably enhanced by the HA coating through AD.

Osteoconductive hydroxyapatite coated PEEK for spinal fusion surgery

Science.gov (United States)

Hahn, Byung-Dong; Park, Dong-Soo; Choi, Jong-Jin; Ryu, Jungho; Yoon, Woon-Ha; Choi, Joon-Hwan; Kim, Jong-Woo; Ahn, Cheol-Woo; Kim, Hyoun-Ee; Yoon, Byung-Ho; Jung, In-Kwon

2013-10-01

Polyetheretherketone (PEEK) has attracted much interest as biomaterial for interbody fusion cages due to its similar stiffness to bone and good radio-transparency for post-op visualization. Hydroxyapatite (HA) coating stimulates bone growth to the medical implant. The objective of this work is to make an implant consisting of biocompatible PEEK with an osteoconductive HA surface for spinal or orthopedic applications. Highly dense and well-adhered HA coating was developed on medical-grade PEEK using aerosol deposition (AD) without thermal degradation of the PEEK. The HA coating had a dense microstructure with no cracks or pores, and showed good adhesion to PEEK at adhesion strengths above 14.3 MPa. The crystallinity of the HA coating was remarkably enhanced by hydrothermal annealing as post-deposition heat-treatment. In addition, in vitro and in vivo biocompatibility of PEEK, in terms of cell adhesion morphology, cell proliferation, differentiation, and bone-to-implant contact ratio, were remarkably enhanced by the HA coating through AD.

In vitro corrosion and cytocompatibility properties of nano-whisker hydroxyapatite coating on magnesium alloy for bone tissue engineering applications.

Science.gov (United States)

Yang, Huawei; Yan, Xueyu; Ling, Min; Xiong, Zuquan; Ou, Caiwen; Lu, Wei

2015-03-17

We report here the successful fabrication of nano-whisker hydroxyapatite (nHA) coatings on Mg alloy by using a simple one-step hydrothermal process in aqueous solution. The nHA coating shows uniform structure and high crystallinity. Results indicate that nHA coating is promising for improving the in vitro corrosion and cytocompatibility properties of Mg-based implants and devices for bone tissue engineering. In addition, the simple hydrothermal deposition method used in the current study is also applicable to substrates with complex shapes or surface geometries.

Effect of Zn{sup 2+}, Fe{sup 3+} and Cr{sup 3+} addition to hydroxyapatite for its application as an active constituent of sunscreens

Energy Technology Data Exchange (ETDEWEB)

De Araujo, T S; De Souza, S O; De Sousa, E M B, E-mail: tatiana.araujo@cefetse.edu.b

2010-11-01

Biocompatible phosphate materials are used in different applications like bone and dental implants, drug delivery systems and others, but could also be applied in inorganic sunscreens. Using sunscreens is extremely necessary, because long time exposure to sun can cause skin cancer. In this work chemical precipitation method has been used to produce hydroxyapatite. Cr{sup 3+}, Zn{sup 2+} and Fe{sup 3+} doped samples were characterized using powder X-Ray Diffraction (XRD) and Optical Absorption techniques. X-ray diffraction measurements confirmed the materials were in the expected crystalline structures. The crystallite size as measured from the X-ray pattern was 23-27 nm ({+-}1). The absorption spectra in the ultraviolet and visible ranges indicate that appropriately doped and sized hydroxyapatite particles may have potential applications as active constituents of sunscreens.

Nanocrystallinity effects on osteoblast and osteoclast response to silicon substituted hydroxyapatite.

Science.gov (United States)

Casarrubios, Laura; Matesanz, María Concepción; Sánchez-Salcedo, Sandra; Arcos, Daniel; Vallet-Regí, María; Portolés, María Teresa

2016-11-15

Silicon substituted hydroxyapatites (SiHA) are highly crystalline bioceramics treated at high temperatures (about 1200°C) which have been approved for clinical use with spinal, orthopedic, periodontal, oral and craniomaxillofacial applications. The preparation of SiHA with lower temperature methods (about 700°C) provides nanocrystalline SiHA (nano-SiHA) with enhanced bioreactivity due to higher surface area and smaller crystal size. The aim of this study has been to know the nanocrystallinity effects on the response of both osteoblasts and osteoclasts (the two main cell types involved in bone remodelling) to silicon substituted hydroxyapatite. Saos-2 osteoblasts and osteoclast-like cells (differentiated from RAW-264.7 macrophages) have been cultured on the surface of nano-SiHA and SiHA disks and different cell parameters have been evaluated: cell adhesion, proliferation, viability, intracellular content of reactive oxygen species, cell cycle phases, apoptosis, cell morphology, osteoclast-like cell differentiation and resorptive activity. This comparative in vitro study evidences that nanocrystallinity of SiHA affects the cell/biomaterial interface inducing bone cell apoptosis by loss of cell anchorage (anoikis), delaying osteoclast-like cell differentiation and decreasing the resorptive activity of this cell type. These results suggest the potential use of nano-SiHA biomaterial for preventing bone resorption in treatment of osteoporotic bone. Copyright © 2016 Elsevier Inc. All rights reserved.

Bone regeneration based on nano-hydroxyapatite and hydroxyapatite/chitosan nanocomposites: an in vitro and in vivo comparative study

International Nuclear Information System (INIS)

Tavakol, S.; Nikpour, M. R.; Amani, A.; Soltani, M.; Rabiee, S. M.; Rezayat, S. M.; Chen, P.; Jahanshahi, M.

2013-01-01

Surface morphology, surface wettability, and size distribution of biomaterials affect their in vitro and in vivo bone regeneration potential. Since nano-hydroxyapatite has a great chemical and structural similarity to natural bone and dental tissues, incorporated biomaterial of such products could improve bioactivity and bone bonding ability. In this research, nano-hydroxyapatite (23 ± 0.09 nm) and its composites with variety of chitosan content [2, 4, and 6 g (45 ± 0.19, 32 ± 0.12, and 28 ± 0.12 nm, respectively)] were prepared via an in situ hybridization route. Size distribution of the particles, protein adsorption, and calcium deposition of powders by the osteoblast cells, gene expression and percentage of new bone formation area were investigated. The highest degree of bone regeneration potential was observed in nano-hydroxyapatite powder, while the bone regeneration was lowest in nano-hydroxyapatite with 6 g of chitosan. Regarding these data, suitable size distribution next to size distribution of hydroxyapatite in bone, smaller size, higher wettability, lower surface roughness of the nano-hydroxyapatite particles and homogeneity in surface resulted in higher protein adsorption, cell differentiation and percentage of bone formation area. Results obtained from in vivo and in vitro tests confirmed the role of surface morphology, surface wettability, mean size and size distribution of biomaterial besides surface chemistry as a temporary bone substitute.

Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold.

Science.gov (United States)

Ciobanu, Gabriela; Ilisei, Simona; Luca, Constantin

2014-02-01

The present paper is focused on a study regarding the possibility of obtaining hydroxyapatite-silver nanoparticle coatings on porous polyurethane scaffold. The method applied is based on a combined strategy involving hydroxyapatite biomimetic deposition on polyurethane surface using a Supersaturated Calcification Solution (SCS), combined with silver ions reduction and in-situ crystallization processes on hydroxyapatite-polyurethane surface by sample immersing in AgNO3 solution. The morphology, composition and phase structure of the prepared samples were characterized by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS) measurements. The data obtained show that a layer of hydroxyapatite was deposited on porous polyurethane support and the silver nanoparticles (average size 34.71 nm) were dispersed among and even on the hydroxyapatite crystals. Hydroxyapatite/polyurethane surface acts as a reducer and a stabilizing agent for silver ions. The surface plasmon resonance peak in UV-Vis absorption spectra showed an absorption maximum at 415 nm, indicating formation of silver nanoparticles. The hydroxyapatite-silver polyurethane scaffolds were tested against Staphylococcus aureus and Escherichia coli and the obtained data were indicative of good antibacterial properties of the materials. © 2013.

In situ synthesis carbonated hydroxyapatite layers on enamel slices with acidic amino acids by a novel two-step method

International Nuclear Information System (INIS)

Wu, Xiaoguang; Zhao, Xu; Li, Yi; Yang, Tao; Yan, Xiujuan; Wang, Ke

2015-01-01

In situ fabrication of carbonated hydroxyapatite (CHA) remineralization layer on an enamel slice was completed in a novel, biomimetic two-step method. First, a CaCO 3 layer was synthesized on the surface of demineralized enamel using an acidic amino acid (aspartic acid or glutamate acid) as a soft template. Second, at the same concentration of the acidic amino acid, rod-like carbonated hydroxyapatite was produced with the CaCO 3 layer as a sacrificial template and a reactant. The morphology, crystallinity and other physicochemical properties of the crystals were characterized using field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrometry (FTIR), X-ray diffraction (XRD) and energy-dispersive X-ray analysis (EDAX), respectively. Acidic amino acid could promote the uniform deposition of hydroxyapatite with rod-like crystals via absorption of phosphate and carbonate ions from the reaction solution. Moreover, compared with hydroxyapatite crystals coated on the enamel when synthesized by a one-step method, the CaCO 3 coating that was synthesized in the first step acted as an active bridge layer and sacrificial template. It played a vital role in orienting the artificial coating layer through the template effect. The results show that the rod-like carbonated hydroxyapatite crystals grow into bundles, which are similar in size and appearance to prisms in human enamel, when using the two-step method with either aspartic acid or acidic glutamate (20.00 mmol/L). - Graphical abstract: FESEM images of enamel slices etched for 60 s and repaired by the two-step method with Glu concentration of 20.00 mmol/L. (A) The boundary (dotted line) of the repaired areas (b) and unrepaired areas (a). (Some selected areas of etched enamel slices were coated with a nail polish before the reaction, which was removed by acetone after the reaction); (B) high magnification image of Ga, (C) high magnification image of Gb. In situ fabrication of carbonated

In situ synthesis carbonated hydroxyapatite layers on enamel slices with acidic amino acids by a novel two-step method

Energy Technology Data Exchange (ETDEWEB)

Wu, Xiaoguang [Department of Pediatric Dentistry, The Hospital of Stomatology, Jilin University, Changchun 130021 (China); Zhao, Xu [College of Chemistry, Jilin University, Changchun 130021 (China); Li, Yi, E-mail: lyi99@jlu.edu.cn [Department of Pediatric Dentistry, The Hospital of Stomatology, Jilin University, Changchun 130021 (China); Yang, Tao [Department of Stomatology, Children' s Hospital of Changchun, 130051 (China); Yan, Xiujuan; Wang, Ke [Department of Pediatric Dentistry, The Hospital of Stomatology, Jilin University, Changchun 130021 (China)

2015-09-01

In situ fabrication of carbonated hydroxyapatite (CHA) remineralization layer on an enamel slice was completed in a novel, biomimetic two-step method. First, a CaCO{sub 3} layer was synthesized on the surface of demineralized enamel using an acidic amino acid (aspartic acid or glutamate acid) as a soft template. Second, at the same concentration of the acidic amino acid, rod-like carbonated hydroxyapatite was produced with the CaCO{sub 3} layer as a sacrificial template and a reactant. The morphology, crystallinity and other physicochemical properties of the crystals were characterized using field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrometry (FTIR), X-ray diffraction (XRD) and energy-dispersive X-ray analysis (EDAX), respectively. Acidic amino acid could promote the uniform deposition of hydroxyapatite with rod-like crystals via absorption of phosphate and carbonate ions from the reaction solution. Moreover, compared with hydroxyapatite crystals coated on the enamel when synthesized by a one-step method, the CaCO{sub 3} coating that was synthesized in the first step acted as an active bridge layer and sacrificial template. It played a vital role in orienting the artificial coating layer through the template effect. The results show that the rod-like carbonated hydroxyapatite crystals grow into bundles, which are similar in size and appearance to prisms in human enamel, when using the two-step method with either aspartic acid or acidic glutamate (20.00 mmol/L). - Graphical abstract: FESEM images of enamel slices etched for 60 s and repaired by the two-step method with Glu concentration of 20.00 mmol/L. (A) The boundary (dotted line) of the repaired areas (b) and unrepaired areas (a). (Some selected areas of etched enamel slices were coated with a nail polish before the reaction, which was removed by acetone after the reaction); (B) high magnification image of Ga, (C) high magnification image of Gb. In situ fabrication of

Synthesis of nanocrystalline hydroxyapatite by using precipitation method

International Nuclear Information System (INIS)

Mobasherpour, I.; Heshajin, M. Soulati; Kazemzadeh, A.; Zakeri, M.

2007-01-01

In this investigation, hydroxyapatite powder has been synthesized from the calcium nitrate hydrated and di-ammonium hydrogen phosphate solution by precipitation method and heat treatment of hydroxyapatite powders. In order to study the structural evolution, the Fourier transform infrared spectroscopy (FTIR), the X-ray diffraction (XRD) and simultaneous thermal analysis (STA) were used. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used to estimate the particle size of the powder and observe the morphology and agglomeration state of the powder. Results show that hydroxyapatite nanocrystalline can successfully be produced by precipitation technique from raw materials. Hydroxyapatite grain gradually increased in size when temperature increased from 100 to 1200 o C, and the hydroxyapatite hexagonal-dipyramidal phase was not transformed to the other calcium phosphates phases up to 1200 o C

Study of sorption processes of strontium on the synthetic hydroxyapatite

International Nuclear Information System (INIS)

Rosskopfova, O.; Galambos, M.; Rajec, P.

2011-01-01

The sorption of strontium on synthetic hydroxyapatite was investigated using batch method and radiotracer technique. The hydroxyapatite samples were prepared by a wet precipitation process followed by calcination of calcium phosphate that precipitated from aqueous solution. Also, commercial hydroxyapatites were used. The sorption of strontium on hydroxyapatite depended on the method of preparation and it was pH independent ranging from 4 to 9 as a result of buffering properties of hydroxyapatite. The distribution coefficient K d was significantly decreased with increasing concentration of Sr 2+ and Ca 2+ ions in solution with concentration above 1 x 10 -3 mol dm -3 . The percentage strontium sorption for commercial and by wet method prepared hydroxyapatite was in the range of 83-96%, while calcined hydroxyapatite was ranging from 10 to 30%. The experimental data for sorption of strontium have been interpreted in the term of Langmuir isotherm. The sorption of Sr 2+ ions was performed by ion-exchange with Ca 2+ cations on the crystal surface of hydroxyapatite. Although calcined hydroxyapatite is successfully used as biomaterial for hard tissues repair, it is not used for the treatment of liquid wastes. (author)

Hydroxyapatite thin films grown by pulsed laser deposition and matrix assisted pulsed laser evaporation: Comparative study

Science.gov (United States)

Popescu-Pelin, G.; Sima, F.; Sima, L. E.; Mihailescu, C. N.; Luculescu, C.; Iordache, I.; Socol, M.; Socol, G.; Mihailescu, I. N.

2017-10-01

Pulsed Laser Deposition (PLD) and Matrix Assisted Pulsed Laser Evaporation (MAPLE) techniques were applied for growing hydroxyapatite (HA) thin films on titanium substrates. All experiments were conducted in a reaction chamber using a KrF* excimer laser source (λ = 248 nm, τFWHM ≈ 25 ns). Half of the samples were post-deposition thermally treated at 500 °C in a flux of water vapours in order to restore crystallinity and improve adherence. Coating surface morphologies and topographies specific to the deposition method were evidenced by scanning electron, atomic force microscopy investigations and profilometry. They were shown to depend on deposition technique and also on the post-deposition treatment. Crystalline structure of the coatings evaluated by X-ray diffraction was improved after thermal treatment. Biocompatibility of coatings, cellular adhesion, proliferation and differentiation tests were conducted using human mesenchymal stem cells (MSCs). Results showed that annealed MAPLE deposited HA coatings were supporting MSCs proliferation, while annealed PLD obtained films were stimulating osteogenic differentiation.

In vitro precipitation of electrodeposited calcium-deficient hydroxyapatite coatings on Ti6Al4V substrate

International Nuclear Information System (INIS)

Dumelie, N.; Benhayoune, H.; Richard, D.; Laurent-Maquin, D.; Balossier, G.

2008-01-01

In this study, electrodeposited calcium phosphate coatings were characterized by X-ray diffraction, using a scanning electron microscope equipped with an EDAX detector, before and after immersion in DMEM (Dulbecco's Modified Eagle Medium). After 1, 7, 14, and 21 days of immersion, the calcium and phosphate contents in solution were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES). The results indicated that precipitation of the coating occurred. Before immersion in DMEM, the electrodeposited coating was a mixed crystalline and amorphous calcium-deficient hydroxyapatite with a Ca/P atomic ratio of about 1.5, but during the immersion period these phases rapidly disappeared and were followed by the precipitation of a crystalline apatite with a Ca/P atomic ratio near 1.65. On the basis of these results, we conclude that an electrodeposited calcium phosphate coating on roughened titanium alloy substrate may act as a precursor for newly precipitated calcium phosphate in in vitro experiments independent of cellular activities

Cytotoxic evaluation of hydroxyapatite-filled and silica/hydroxyapatite-filled acrylate-based restorative composite resins: An in vitro study.

Science.gov (United States)

Chadda, Harshita; Naveen, Sangeetha Vasudevaraj; Mohan, Saktiswaren; Satapathy, Bhabani K; Ray, Alok R; Kamarul, Tunku

2016-07-01

Although the physical and mechanical properties of hydroxyapatite-filled dental restorative composite resins have been examined, the biocompatibility of these materials has not been studied in detail. The purpose of this in vitro study was to analyze the toxicity of acrylate-based restorative composite resins filled with hydroxyapatite and a silica/hydroxyapatite combination. Five different restorative materials based on bisphenol A-glycidyl methacrylate (bis-GMA) and tri-ethylene glycol dimethacrylate (TEGDMA) were developed: unfilled (H0), hydroxyapatite-filled (H30, H50), and silica/hydroxyapatite-filled (SH30, SH50) composite resins. These were tested for in vitro cytotoxicity by using human bone marrow mesenchymal stromal cells. Surface morphology, elemental composition, and functional groups were determined by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), and Fourier-transformed infrared spectroscopy (FTIR). The spectra normalization, baseline corrections, and peak integration were carried out by OPUS v4.0 software. Both in vitro cytotoxicity results and SEM analysis indicated that the composite resins developed were nontoxic and supported cell adherence. Elemental analysis with EDX revealed the presence of carbon, oxygen, calcium, silicon, and gold, while the presence of methacrylate, hydroxyl, and methylene functional groups was confirmed through FTIR analysis. The characterization and compatibility studies showed that these hydroxyapatite-filled and silica/hydroxyapatite-filled bis-GMA/TEGDMA-based restorative composite resins are nontoxic to human bone marrow mesenchymal stromal cells and show a favorable biologic response, making them potential biomaterials. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Structure and characteristics of the hot pressed hydroxyapatite/poly-L-lactide composite

Directory of Open Access Journals (Sweden)

Ignjatović Nenad L.

2002-01-01

Full Text Available Hydroxyapatite/poly-L-lactide (HAp/PLL composite biomaterial can be obtained by different processing methods. Three-dimensional blocks of HAp/PLLA composite biomaterial with mechanical characteristics close to the natural bone tissue can be obtained by hot pressing procedure. Effects of synthesis and compacting on the structure and characteristics of the HAp/PLLA composite biomaterial were studied in this work. Using wade angle X-ray structural analyses (WAXS, differentially scanning calorimetry (DSC, thermogravimetric analysis (TGA and infrared (IR spectroscopy, the changes occurring in the material during synthesis and hot pressing were monitored. Surface microstructure was analyzed by scanning electronic microscopy (SEM coupled with electron-dispersion analysis (EDX. The results obtained indicate a possible decrease in the degree of crystallinity with hot pressing time increase. A block of HAp/PLLA composite biomaterial with 1.6 times lower crystallinity of the polymer phase was obtained by hot pressing in a given time interval with a maximum of 60 minutes. Results of TG analysis show that PLLA stability decreases with increasing hot pressing time, and vice versa. IR study proved that neither destructive changes in constituents nor formation of new phases occurred during hot pressing.

RF Magnetron Sputtering Coating Of Hydroxyapatite On Alkali Solution Treated Titanate Nanorods

Directory of Open Access Journals (Sweden)

Lee K.

2015-06-01

Full Text Available Hydroxyapatite (HA is a material with outstanding biocompatibility. It is chemically similar to natural bone tissue, and has therefore been favored for use as a coating material for dental and orthopedic implants. In this study, RF magnetron sputtering was applied for HA coating. And Alkali treatment was performed in a 5 M NaOH solution at 60°C. The coated HA thin film was heat-treated at a range of temperatures from 300 to 600°C. The morphological characterization and crystal structures of the coated specimens were then obtained via FE-SEM, XRD, and FT-IR. The amorphous thin film obtained on hydrothermally treated nanorods transformed into a crystalline thin film after the heat treatment. The change in the phase transformation, with an enhanced crystallinity, showed a reduced wettability. The hydrothermally treated nanorods with an amorphous thin film, on the other hand, showed an outstanding wettability. The HA thin film perpendicularly coated the nanorods in the upper and inner parts via RF magnetron sputtering, and the FT-IR results confirmed that the molecular bonding of the coated film had an HA structure.

Bacterial Cellulose-Hydroxyapatite Nanocomposites for Bone Regeneration

Directory of Open Access Journals (Sweden)

S. Saska

2011-01-01

Full Text Available The aim of this study was to develop and to evaluate the biological properties of bacterial cellulose-hydroxyapatite (BC-HA nanocomposite membranes for bone regeneration. Nanocomposites were prepared from bacterial cellulose membranes sequentially incubated in solutions of CaCl2 followed by Na2HPO4. BC-HA membranes were evaluated in noncritical bone defects in rat tibiae at 1, 4, and 16 weeks. Thermogravimetric analyses showed that the amount of the mineral phase was 40%–50% of the total weight. Spectroscopy, electronic microscopy/energy dispersive X-ray analyses, and X-ray diffraction showed formation of HA crystals on BC nanofibres. Low crystallinity HA crystals presented Ca/P a molar ratio of 1.5 (calcium-deficient HA, similar to physiological bone. Fourier transformed infrared spectroscopy analysis showed bands assigned to phosphate and carbonate ions. In vivo tests showed no inflammatory reaction after 1 week. After 4 weeks, defects were observed to be completely filled in by new bone tissue. The BC-HA membranes were effective for bone regeneration.

Facile fabrication of bioactive ultra-small protein–hydroxyapatite nanoconjugates via liquid-phase laser ablation and their enhanced osteogenic differentiation activity

KAUST Repository

Rodio, Marina; Coluccino, Luca; Romeo, Elisa; Genovese, Alessandro; Diaspro, Alberto; Garau, Gianpiero; Intartaglia, Romuald

2016-01-01

Hydroxyapatite bioactive complexes are being increasingly recognized as effective available means in regenerative medicine. Conventional technologies for their synthesis have drawbacks from a synthetic standpoint, mainly requiring high temperatures and multi-step processes. Here, we show that ultra-small hydroxyapatite conjugated-nanoparticles (Ha-CNPs) can be obtained at room temperature by Pulsed Laser Ablation (PLA) directly in protein solution using picosecond pulses at near infrared wavelengths. The results showed that the nanoparticle size was driven by the concentration of the protein. Using this approach, we obtained aqueous soluble and ultra-small crystalline nanoparticles of ≈3 nm diameter coated with protein molecules (surface coverage ≈ 5.5 pmol cm; zeta potential ≈-33.5 mV). These nanoparticles showed low cytotoxicity in vitro compared to chemically synthesized nanoparticles, and revealed proliferative and osteoinductive effects on human bone marrow mesenchymal stem cells (hMSCs). The resulting enhanced cell osteogenic differentiation suggested that our PLA-based synthetic approach might be exploited in novel applications of regenerative medicine.

Facile fabrication of bioactive ultra-small protein–hydroxyapatite nanoconjugates via liquid-phase laser ablation and their enhanced osteogenic differentiation activity

KAUST Repository

Rodio, Marina

2016-11-24

Hydroxyapatite bioactive complexes are being increasingly recognized as effective available means in regenerative medicine. Conventional technologies for their synthesis have drawbacks from a synthetic standpoint, mainly requiring high temperatures and multi-step processes. Here, we show that ultra-small hydroxyapatite conjugated-nanoparticles (Ha-CNPs) can be obtained at room temperature by Pulsed Laser Ablation (PLA) directly in protein solution using picosecond pulses at near infrared wavelengths. The results showed that the nanoparticle size was driven by the concentration of the protein. Using this approach, we obtained aqueous soluble and ultra-small crystalline nanoparticles of ≈3 nm diameter coated with protein molecules (surface coverage ≈ 5.5 pmol cm; zeta potential ≈-33.5 mV). These nanoparticles showed low cytotoxicity in vitro compared to chemically synthesized nanoparticles, and revealed proliferative and osteoinductive effects on human bone marrow mesenchymal stem cells (hMSCs). The resulting enhanced cell osteogenic differentiation suggested that our PLA-based synthetic approach might be exploited in novel applications of regenerative medicine.

In Vitro Corrosion and Cytocompatibility Properties of Nano-Whisker Hydroxyapatite Coating on Magnesium Alloy for Bone Tissue Engineering Applications

Directory of Open Access Journals (Sweden)

Huawei Yang

2015-03-01

Full Text Available We report here the successful fabrication of nano-whisker hydroxyapatite (nHA coatings on Mg alloy by using a simple one-step hydrothermal process in aqueous solution. The nHA coating shows uniform structure and high crystallinity. Results indicate that nHA coating is promising for improving the in vitro corrosion and cytocompatibility properties of Mg-based implants and devices for bone tissue engineering. In addition, the simple hydrothermal deposition method used in the current study is also applicable to substrates with complex shapes or surface geometries.

Fabrication of palladium nanoparticles immobilized on an amine-functionalized ceramic membrane support using a nanoparticulate colloidal impregnation method with enhanced catalytic properties

Energy Technology Data Exchange (ETDEWEB)

Du, Yan; Chen, Rizhi [Nanjing Tech University, Nanjing (China)

2015-09-15

An efficient and reusable catalyst was developed by depositing palladium nanoparticles on an amine-functionalized ceramic membrane support using a nanoparticulate colloidal impregnation method. The as-prepared Pdloaded ceramic membrane support was characterized by XRD, SEM, EDS, TEM, XPS, ICP, and its catalytic properties were investigated in the liquid-phase p-nitrophenol hydrogenation. A comparative study was also made with the palladium nanoparticles deposited on an amine-functionalized ceramic membrane support by an impregnation-reduction method. The palladium nanoparticles could be homogeneously immobilized on the ceramic membrane support surface, and exhibited excellent catalytic performance in the p-nitrophenol hydrogenation. The catalytic activity of the Pdloaded ceramic membrane support prepared by the nanoparticulate colloidal impregnation method increased by 16.6% compared to that of impregnation-reduction method. In the nanoparticulate colloidal impregnation method, palladium nanoparticles were presynthesized, higher loading of Pd(0) could be obtained, resulting in better catalytic activity. The as-prepared Pd-loaded ceramic membrane support could be easily reused for several cycles without appreciable degradation of catalytic activity.

The infrared spectroscopy in the study of the bone crystallinity thermally affected; La espectroscopia infrarroja en el estudio de la cristalinidad del hueso afectado termicamente

Energy Technology Data Exchange (ETDEWEB)

Medina, C.; Tiesler, V. [Universidad Autonoma de Yucatan, Facultad de Ciencias Antropoloicas. 97000 Merida, Yucatan (Mexico); Azamar, J.A.; Alvarado G, J.J.; Quintana, P. [CINVESTAV-Unidad Merida, Depto. Fisica Aplicada, Km 6 Ant. Carr. a Progreso, 97310 Merida, Yucatan (Mexico)

2006-07-01

Bone is made up by both organic and inorganic components. Among the latter stands out hydroxyapatite (HAP), composed by hexagonal crystallites arranged in a laminar form. The size of the hydroxyapatite crystals may be altered by different conditions, among those figures thermal exhibition, since during burning the bone eliminates organic matrix and thus promotes the crystallization process of the material. An experimental series was designed to measure crystallinity, in which pig bone remains were burnt at different temperatures and analyzed by infrared spectroscopy (FTIR). By means of analogy a comparison was made between the infrared spectra in order to compare with the ones obtained from the archaeological samples, coming from the Classic period Maya sites of Calakmul and Becan, Campeche. (Author)

Formation of Biomimetic Hydroxyapatite Coating on Titanium Plates

Directory of Open Access Journals (Sweden)

Ievgen Volodymyrovych PYLYPCHUK

2014-09-01

Full Text Available Hydroxyapatite (HA has long been used as a coating material in the implant industry for orthopedic implant applications. HA is the natural inorganic constituent of bone and teeth. By coating titanium (base material of implant engineering because of its lightness and durability with hydroxyapatite, we can provide higher biocompatibility of titanium implants, according to HA ability to form a direct biochemical bond with living tissues. This article reports a biomimetic approach for coating hydroxyapatite with titanium A method of modifying the surface of titanium by organic modifiers (for creating functional groups on the surface, followed by formation "self-assembled" layer of biomimetic hydroxyapatite in simulated body fluid (SBF. FTIR and XPS confirmed the formation of hydroxyapatite coatings on titanium surface. Comparative study of the formation of HA on the surface of titanium plates modified by different functional groups: Ti(≡OH, Ti/(≡Si-OH and Ti/(≡COOH is conducted. It was found that the closest to natural stoichiometric hydroxyapatite Ca/P ratio was obtained on Ti/(≡COOH samples. DOI: http://dx.doi.org/10.5755/j01.ms.20.3.4974

Ferroelectric Polarization in Nanocrystalline Hydroxyapatite Thin Films on Silicon

Science.gov (United States)

Lang, S. B.; Tofail, S. A. M.; Kholkin, A. L.; Wojtaś, M.; Gregor, M.; Gandhi, A. A.; Wang, Y.; Bauer, S.; Krause, M.; Plecenik, A.

2013-01-01

Hydroxyapatite nanocrystals in natural form are a major component of bone- a known piezoelectric material. Synthetic hydroxyapatite is widely used in bone grafts and prosthetic pyroelectric coatings as it binds strongly with natural bone. Nanocrystalline synthetic hydroxyapatite films have recently been found to exhibit strong piezoelectricity and pyroelectricity. While a spontaneous polarization in hydroxyapatite has been predicted since 2005, the reversibility of this polarization (i.e. ferroelectricity) requires experimental evidence. Here we use piezoresponse force microscopy to demonstrate that nanocrystalline hydroxyapatite indeed exhibits ferroelectricity: a reversal of polarization under an electrical field. This finding will strengthen investigations on the role of electrical polarization in biomineralization and bone-density related diseases. As hydroxyapatite is one of the most common biocompatible materials, our findings will also stimulate systematic exploration of lead and rare-metal free ferroelectric devices for potential applications in areas as diverse as in vivo and ex vivo energy harvesting, biosensing and electronics. PMID:23884324

Synthesis and characterization of praseodymium-142 hydroxyapatite (142Pr-HA)

International Nuclear Information System (INIS)

Duyeh Setiawan; Daud Nurhasan

2015-01-01

The use of radioisotope of lanthanide group with range of beta energy 0.4 - 2.2 MeV has been renewed interest in nuclear medicine. Praseodymium-142 radioisotope ( 142 Pr, t 1/2 = 19.2 hours, E β = 2.16 MeV) is suitable for applications radiotherapy. Labelled of the hydroxyapatite (Ca 10 (PO 4 )6(OH) 2 ) can be used as carrier of radionuclide after injection in the body injection. This research aim as a preliminary studies to make praseodymium-142 hydroxyapatite ( 142 Pr-HA) as a radiotherapy agent. The optimum condition of praseodymium-142 hydroxyapatite synthesis by controlling several parameters such as the pH and the weight of hydroxyapatite was obtained from process by used the nonradioactive praseodymium. The optimum condition of hydroxyapatite by praseodymium are at pH 5 and weight ratio praseodymium : hydroxyapatite is 1 : 16. The percentage of labeling hydroxyapatite with 142 PrCl 3 was 99.50% and the radiochemical purity of 142 Pr-Ha was 95.20%. (author)

Properties and in vivo investigation of nanocrystalline hydroxyapatite obtained by mechanical alloying

Energy Technology Data Exchange (ETDEWEB)

Silva, C.C.; Pinheiro, A.G.; Oliveira, R.S. de; Goes, J.C.; Aranha, N.; Oliveira, L.R. de; Sombra, A.S.B

2004-06-01

Mechanical alloying has been used successfully to produce nanocrystalline powders of hydroxyapatite (HA) using three different procedures. The milled HA was studied by X-ray diffraction, Infrared, Raman scattering spectroscopy and Scanning Electron Microscopy (SEM). We obtained HA with different degrees of crystallinity and time of milling. The grain size analysis through SEM and XRD shows particles with dimensions of 36.9, 14.3 and 35.5 nm (for (R1), (R2) and (R3), respectively) forming bigger units with dimensions given by 117.2, 110.8 and 154.4 nm (for (R1), (R2) and (R3), respectively). The Energy-Dispersive Spectroscopy (EDS) analysis showed that an atomic ratio of Ca/P=1.67, 1.83 and 1.50 for reactions (R1), (R2) and (R3), respectively. These results suggest that the R1 nanocrystalline ceramic is closer to the expected value for the ratio Ca/P for hydroxyapatite, which is 5/3 congruent with 1.67. The bioactivity analysis shows that all the samples implanted into the rabbits can be considered biocompatible, since they had been considered not toxic, had not caused inflammation and reject on the part of the organisms of the animals, during the period of implantation. The samples implanted in rabbits had presented new osseous tissue formation with the presence of osteoblasts cells.

Properties and in vivo investigation of nanocrystalline hydroxyapatite obtained by mechanical alloying

International Nuclear Information System (INIS)

Silva, C.C.; Pinheiro, A.G.; Oliveira, R.S. de; Goes, J.C.; Aranha, N.; Oliveira, L.R. de; Sombra, A.S.B.

2004-01-01

Mechanical alloying has been used successfully to produce nanocrystalline powders of hydroxyapatite (HA) using three different procedures. The milled HA was studied by X-ray diffraction, Infrared, Raman scattering spectroscopy and Scanning Electron Microscopy (SEM). We obtained HA with different degrees of crystallinity and time of milling. The grain size analysis through SEM and XRD shows particles with dimensions of 36.9, 14.3 and 35.5 nm (for (R1), (R2) and (R3), respectively) forming bigger units with dimensions given by 117.2, 110.8 and 154.4 nm (for (R1), (R2) and (R3), respectively). The Energy-Dispersive Spectroscopy (EDS) analysis showed that an atomic ratio of Ca/P=1.67, 1.83 and 1.50 for reactions (R1), (R2) and (R3), respectively. These results suggest that the R1 nanocrystalline ceramic is closer to the expected value for the ratio Ca/P for hydroxyapatite, which is 5/3 congruent with 1.67. The bioactivity analysis shows that all the samples implanted into the rabbits can be considered biocompatible, since they had been considered not toxic, had not caused inflammation and reject on the part of the organisms of the animals, during the period of implantation. The samples implanted in rabbits had presented new osseous tissue formation with the presence of osteoblasts cells

Factors influencing the deposition of hydroxyapatite coating onto hollow glass microspheres

International Nuclear Information System (INIS)

Jiao, Yan; Xiao, Gui-Yong; Xu, Wen-Hua; Zhu, Rui-Fu; Lu, Yu-Peng

2013-01-01

Hydroxyapatite (HA) and HA coated microcarriers for cell culture and delivery have attracted more attention recently, owing to the rapid progress in the field of tissue engineering. In this research, a dense and uniform HA coating with the thickness of about 2 μm was successfully deposited on hollow glass microspheres (HGM) by biomimetic process. The influences of SBF concentration, immersion time, solid/liquid ratio and activation of HGM on the deposition rate and coating characteristics were discussed. X-ray diffraction (XRD) and Fourier transform infrared spectrum (FTIR) analyses revealed that the deposited HA is poorly crystalline. The thickness of HA coating showed almost no increase after immersion in 1.5SBF for more than 15 days with the solid/liquid ratio of 1:150. At the same time, SBF concentration, solid/liquid ratio and activation treatment played vital roles in the formation of HA coating on HGM. This poorly crystallized HA coated HGM could have potential use as microcarrier for cell culture. Highlights: • HA coatings were deposited on hollow glass microspheres by biomimetic process. • The obtained HA coating was poorly crystalline and carbonated. • The influencing factors of deposition rate and coating characteristics were studied. • The thickness of HA coating showed almost no increase after immersion for 15 days

Variation de la composition de nanoparticules de 1-10 nm obtenues par séparation de phase dans un verre de silice

OpenAIRE

Blanc , W; Francois-Saint-Cyr , H; Martin , I; Lecoustumer , P; Hombourger , C; R. Neuville , D.; Larson , D.J.; Prosa , T.J.; Guillermier , C

2014-01-01

National audience; Les verres contenant des nanoparticules ont de nombreuses applications industrielles, notamment grâce à leurs excellentes propriétés thermo-mécaniques [1]. Ils présentent aussi un intérêt pour les propriétés optiques. En effet, l'encapsulation d'ions luminescents (ions de terre rare par exemple) dans des nanoparticules entraînent de nouvelles propriétés de luminescence qui n'existeraient pas dans le verre hôte (bande d'émission élargie, efficacité quantique augmentée, etc) ...

Fabrication, ultra-structure characterization and in vitro studies of RF magnetron sputter deposited nano-hydroxyapatite thin films for biomedical applications

Science.gov (United States)

Surmeneva, Maria A.; Surmenev, Roman A.; Nikonova, Yulia A.; Selezneva, Irina I.; Ivanova, Anna A.; Putlyaev, Valery I.; Prymak, Oleg; Epple, Matthias

2014-10-01

A series of nanostructured low-crystalline hydroxyapatite (HA) coatings averaging 170, 250, and 440 nm in thickness were deposited onto previously etched titanium substrates through radio-frequency (RF) magnetron sputtering. The HA coatings were analyzed using infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM). Cross sections of the thin specimens were prepared by FIB to study the microstructure of the coatings by TEM. The deposition process formed nano-scale grains, generating an amorphous layer at the substrate/coating interface and inducing the growth of a columnar grain structure perpendicular to the substrate surface. A microstructural analysis of the film confirmed that the grain size and crystallinity increased when increasing the deposition time. The nanostructured HA coatings were not cytotoxic, as proven by in vitro assays using primary dental pulp stem cells and mouse fibroblast NCTC clone L929 cells. Low-crystallinity HA coatings with different thicknesses stimulated cells to attach, proliferate and form mineralized nodules on the surface better than uncoated titanium substrates.

Sorption of technetium on composite chitosan-hydroxyapatite from aqueous solutions

International Nuclear Information System (INIS)

Pivarciova, L.; Rosskopfova, O.; Galambos, M.; Rajec, P.

2013-01-01

Biomaterials such as natural polymers (chitosan) and hydroxyapatite have an important application in material for bone replacement. Most of chitosan/hydroxyapatite composites are prepared by mixing hydroxyapatite particles with chitosan matrices. Another method of preparation of chitosan/hydroxyapatite composite is in-situ generation of nano-hydroxyapatite in chitosan matrix. The most common biomaterial used in the past years in hard tissue regeneration was hydroxyapatite, owing to its properties as biocompatibility, bioactivity, non-toxicity, non-immunogenicity etc. Chitosan is a polyaminosacharide, partially deacetylated product of chitin. Chitosan can be used in combination with other materials to enhance bone growth such as bone filling paste. The aims of this work were: the influence of the contact time on sorption of pertechnate anions on chitosan/hydroxyapatite composites; the effect of pH on sorption of pertechnate anions on chitosan/hydroxyapatite composites; the effect of foreign ions on sorption of pertechnate anions on chitosan/hydroxyapatite composites. The author concluded: the percentage of technetium sorption after 1 hour of contact time was > 97 %. In the initial pH range of 2.9-10.2, the percentage of technetium sorption on chitosan/hydroxyapatite composites CH/HA(A), CH/HA(B), CH/HA 30:70, ZCH was > 98 % and on CH/HA 50:50 was > 94%. The competition effect of Fe 2+ towards TcO 4 :- sorption is stronger than competition effect of other observed cations for all examined composites with the same weight ratio. The percentage of the technetium sorption was the same for all composites with the weight ratio of 30:70. (authors)

Rapid detection of cancer related DNA nanoparticulate biomarkers and nanoparticles in whole blood

Science.gov (United States)

Heller, Michael J.; Krishnan, Raj; Sonnenberg, Avery

2010-08-01

The ability to rapidly detect cell free circulating (cfc) DNA, cfc-RNA, exosomes and other nanoparticulate disease biomarkers as well as drug delivery nanoparticles directly in blood is a major challenge for nanomedicine. We now show that microarray and new high voltage dielectrophoretic (DEP) devices can be used to rapidly isolate and detect cfc-DNA nanoparticulates and nanoparticles directly from whole blood and other high conductance samples (plasma, serum, urine, etc.). At DEP frequencies of 5kHz-10kHz both fluorescent-stained high molecular weight (hmw) DNA, cfc-DNA and fluorescent nanoparticles separate from the blood and become highly concentrated at specific DEP highfield regions over the microelectrodes, while blood cells move to the DEP low field-regions. The blood cells can then be removed by a simple fluidic wash while the DNA and nanoparticles remain highly concentrated. The hmw-DNA could be detected at a level of <260ng/ml and the nanoparticles at <9.5 x 109 particles/ml, detection levels that are well within the range for viable clinical diagnostics and drug nanoparticle monitoring. Disease specific cfc-DNA materials could also be detected directly in blood from patients with Chronic Lymphocytic Leukemia (CLL) and confirmed by PCR genotyping analysis.

Synthesis and synchrotron characterisation of novel dual-template of hydroxyapatite scaffolds with controlled size porous distribution

Energy Technology Data Exchange (ETDEWEB)

Lima, Thiago A. R. M.; Ilavsky, Jan; Hammons, Joshua; Sarmento, Victor H. V.; Rey, José F. Q.; Valerio, Mário E. G.

2017-03-01

Hydroxyapatite (HAP) scaffolds with a hierarchical porous architecture were prepared by a new dual-template (corn starch and cetyltrimethylammonium bromide (CTAB) surfactant) used to cast HAP nanoparticles and development scaffolds with size hierarchical porous distribution. The Powder X-Ray diffraction (XRD) results showed that only the HAP crystalline phase is present in the samples after calcination; the Scanning Electron Microscopy (SEM) combined with Small Angle (SAXS) and Ultra-Small Angle X-ray Scattering (USAXS) techniques showed that the porous arrangement is promoted by needle-like HAP nanoparticles, and that the pore size distributions depend on the drip-order of the calcium and the phosphate solutions during the template preparation stage.

Characterisation of Suspension Precipitated Nanocrystalline Hydroxyapatite Powders

International Nuclear Information System (INIS)

Mallik, P K; Swain, P.K.; Patnaik, S.C

2016-01-01

Hydroxyapatite (HA) is a well-known biomaterial for coating on femoral implants, filling of dental cavity and scaffold for tissue replacement. Hydroxyapatite possess limited load bearing capacity due to their brittleness. In this paper, the synthesis of nanocrystalline hydroxyapatite powders was prepared by dissolving calcium oxide in phosphoric acid, followed by addition of ammonia liquor in a beaker. The prepared solution was stirred by using magnetic stirrer operated at temperature of 80°C for an hour. This leads to the formation of hydroxyapatite precipitate. The precipitate was dried in oven for overnight at 100°C. The dried agglomerated precipitate was calcined at 800°C in conventional furnace for an hour. The influence of calcium oxide concentration and pH on the resulting precipitates was studied using BET, XRD and SEM. As result, a well-defined sub-rounded morphology of powders size of ∼41 nm was obtained with a salt concentration of 0.02 M. Finally, it can be concluded that small changes in the reaction conditions led to large changes in final size, shape and degree of aggregation of the hydroxyapatite particles. (paper)

Synthesis of calcium hydroxyapatite from calcium carbonate and different orthophosphate sources: A comparative study

International Nuclear Information System (INIS)

Pham Minh, Doan; Lyczko, Nathalie; Sebei, Haroun; Nzihou, Ange; Sharrock, Patrick

2012-01-01

Highlights: ► Calcium hydroxyapatite was synthesized from CaCO 3 and four orthophosphates. ► Only H 3 PO 4 led to the complete precipitation of orthophosphate species. ► H 3 PO 4 was also the most efficient for calcium dissolution. ► Reaction pathway was dissolution-precipitation accompanied by agglomeration step. - Abstract: The synthesis of calcium hydroxyapatite (Ca-HA) starting from calcium carbonate and different orthophosphate sources, including orthophosphoric acid, potassium, sodium and ammonium dihydrogen orthophosphates, was investigated under ambient conditions. The reaction started with calcium carbonate dissolution in an acid medium, followed by rapid precipitation of calcium cations with orthophosphate species to form calcium phosphate based particles which were in the size range of 0.4–1 μm. These particles then agglomerated into much larger ones, up to 350 μm in diameter (aggregates). These aggregates possessed an unstable porous structure which was responsible for the porosity of the final products. The highest specific surface area and pore volume were obtained with potassium dihydrogen orthophosphate. On the other hand, orthophosphoric acid led to the highest dissolution of calcium carbonate and the complete precipitation of orthophosphate species. Under ambient conditions, calcium phosphate based solid products of low crystallinity were formed. Different intermediates were identified and a reaction pathway proposed.

Cadmium immobilization by hydroxyapatite

Directory of Open Access Journals (Sweden)

Smičiklas Ivana D.

2003-01-01

Full Text Available The contamination of air, soil and water by cadmium is a great environmental problem. If cadmium occurs in nature in ionic form, soluble in water, it easily enters into the food chain. Hydroxyapatite (HAP, Ca-o(POAe(OH2 is a sparingly soluble salt and an excellent matrix for the removal of heavy metals from solutions. Considerable research attention has been paid to the bond between Cc/2+ ions and synthetic hydroxyapatite of known composition. The sorption mechanism is complex. The dominant process is ion exchange, but surface adsorption, surface complexation and coprecipitation can also contribute to the overall mechanism. The sorption capacity depends on the characteristics of hydroxyapatite itself and on the experimental conditions. Under optimum conditions a maximum capacity of 0.8 mol Cd2+/mol HAP can be achieved. HAP is a potential sorbent for the remediation of contaminated water and soil, for industrial waste treatment, and it is also referenced as a material that can be used as a barrier around waste depositories.

In situ deposition of hydroxyapatite on graphene nanosheets

International Nuclear Information System (INIS)

Neelgund, Gururaj M.; Oki, Aderemi; Luo, Zhiping

2013-01-01

Graphical abstract: A facile chemical precipitation method is reported for effective in situ deposition of hydroxyapatite on graphene nanosheets. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. Display Omitted Highlights: ► It is a facile and effective method for deposition of HA on GR nanosheets. ► It avoids the use of harmful reducing agents like hydrazine, NaBH 4 etc. ► GR nanosheets were produced using bio-compatible, ethylenediamine. ► The graphitic structure of synthesized GR nanosheets was high ordered. ► The ratio of Ca to P in HA was 1.64, which is close to ratio in natural bone. -- Abstract: Graphene nanosheets were effectively functionalized by in situ deposition of hydroxyapatite through a facile chemical precipitation method. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. The resulting hydroxyapatite functionalized graphene nanosheets were characterized by attenuated total reflection IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray energy dispersive spectroscopy, Raman spectroscopy and thermogravimetric analysis. These characterization techniques revealed the successful grafting of hydroxyapatite over well exfoliated graphene nanosheets without destroying their structure.

In situ deposition of hydroxyapatite on graphene nanosheets

Energy Technology Data Exchange (ETDEWEB)

Neelgund, Gururaj M. [Department of Chemistry, Prairie View A and M University, Prairie View, TX 77446 (United States); Oki, Aderemi, E-mail: aroki@pvamu.edu [Department of Chemistry, Prairie View A and M University, Prairie View, TX 77446 (United States); Luo, Zhiping [Microscopy and Imaging Center and Materials Science and Engineering Program, Texas A and M University, College Station, TX 77843 (United States)

2013-02-15

Graphical abstract: A facile chemical precipitation method is reported for effective in situ deposition of hydroxyapatite on graphene nanosheets. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. Display Omitted Highlights: ► It is a facile and effective method for deposition of HA on GR nanosheets. ► It avoids the use of harmful reducing agents like hydrazine, NaBH{sub 4} etc. ► GR nanosheets were produced using bio-compatible, ethylenediamine. ► The graphitic structure of synthesized GR nanosheets was high ordered. ► The ratio of Ca to P in HA was 1.64, which is close to ratio in natural bone. -- Abstract: Graphene nanosheets were effectively functionalized by in situ deposition of hydroxyapatite through a facile chemical precipitation method. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. The resulting hydroxyapatite functionalized graphene nanosheets were characterized by attenuated total reflection IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray energy dispersive spectroscopy, Raman spectroscopy and thermogravimetric analysis. These characterization techniques revealed the successful grafting of hydroxyapatite over well exfoliated graphene nanosheets without destroying their structure.

The Influence of Spray Parameters on the Characteristics of Hydroxyapatite In-Flight Particles, Splats and Coatings by Micro-plasma Spraying

Science.gov (United States)

Liu, Xiao-mei; He, Ding-yong; Wang, Yi-ming; Zhou, Zheng; Wang, Guo-hong; Tan, Zhen; Wang, Zeng-jie

2018-04-01

Hydroxyapatite (HA) is one of the most important bioceramic materials used in medical implants. The structure of HA coatings is closely related to their manufacturing process. In the present study, HA coatings were deposited on Ti-6Al-4V substrate by micro-plasma spraying. Results show that three distinct HA coatings could be obtained by changing the spraying power from 0.5 to 1.0 kW and spraying stand-off distance from 60 to 110 mm: (1) high crystallinity (93.3%) coatings with porous structure, (2) high crystallinity coatings (86%) with columnar structure, (3) higher amorphous calcium phosphate (ACP, 50%) coatings with dense structure. The in-flight particles melting state and splat topography was analyzed to better understand the formation mechanism of three distinct HA coatings. Results show that HA coatings sprayed at low spraying power and short stand-off distance exhibit high crystallinity and porosity is attributed to the presence of partially melted particles. High crystallinity HA coatings with (002) crystallographic texture could be deposited due to the complete melting of the in-flight particles and low cooling rate of the disk shape splats under higher spraying power and shorter SOD. However, splashed shape splats with relative high cooling can be provided by increasing SOD, which leads to the formation of ACP.

Detection of hydroxyapatite in calcified cardiovascular tissues.

Science.gov (United States)

Lee, Jae Sam; Morrisett, Joel D; Tung, Ching-Hsuan

2012-10-01

The objective of this study is to develop a method for selective detection of the calcific (hydroxyapatite) component in human aortic smooth muscle cells in vitro and in calcified cardiovascular tissues ex vivo. This method uses a novel optical molecular imaging contrast dye, Cy-HABP-19, to target calcified cells and tissues. A peptide that mimics the binding affinity of osteocalcin was used to label hydroxyapatite in vitro and ex vivo. Morphological changes in vascular smooth muscle cells were evaluated at an early stage of the mineralization process induced by extrinsic stimuli, osteogenic factors and a magnetic suspension cell culture. Hydroxyapatite components were detected in monolayers of these cells in the presence of osteogenic factors and a magnetic suspension environment. Atherosclerotic plaque contains multiple components including lipidic, fibrotic, thrombotic, and calcific materials. Using optical imaging and the Cy-HABP-19 molecular imaging probe, we demonstrated that hydroxyapatite components could be selectively distinguished from various calcium salts in human aortic smooth muscle cells in vitro and in calcified cardiovascular tissues, carotid endarterectomy samples and aortic valves, ex vivo. Hydroxyapatite deposits in cardiovascular tissues were selectively detected in the early stage of the calcification process using our Cy-HABP-19 probe. This new probe makes it possible to study the earliest events associated with vascular hydroxyapatite deposition at the cellular and molecular levels. This target-selective molecular imaging probe approach holds high potential for revealing early pathophysiological changes, leading to progression, regression, or stabilization of cardiovascular diseases. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Niobium-Doped Hydroxyapatite Bioceramics: Synthesis, Characterization and In Vitro Cytocompatibility

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Nádia S. V. Capanema

2015-07-01

Full Text Available Doping calcium phosphates with ionic species can play an important role in biological responses promoting alkaline phosphatase activity, and, therefore inducing the generation of new bone. Thus, in this study, the synthesis of niobium-doped hydroxyapatite (Nb-HA nanosize particles obtained by the precipitation process in aqueous media followed by thermal treatment is presented. The bioceramics were extensively characterized by X-ray diffraction, wavelength dispersive X-ray fluorescence spectrometry, Fourier transform infrared spectroscopy, scanning electron microscopy/energy dispersive X-ray spectroscopy analysis, transmission electron microscopy, atomic force microscopy and thermal analysis regarding their chemical composition, structure and morphology. The results showed that the precipitate dried at 110 °C was composed of amorphous calcium phosphate and HA, with polidisperse particles ranging from micro to nano dimensions. After the thermal treatment at 900 °C, the bioceramic system evolved predominantly to HA crystalline phase, with evident features of particle sintering and reduction of surface area. Moreover, the addition of 10 mol% of niobium salt precursor during the synthesis indicated the complete incorporation of the Nb(V species in the HA crystals with detectable changes in the original lattice parameters. Furthermore, the incorporation of Nb ions caused a significant refinement on the average particle size of HA. Finally, the preliminary cytocompatibility response of the biomaterials was accessed by human osteoblast cell culture using MTT and resazurin assays, which demonstrated no cytotoxicity of the Nb-alloyed hydroxyapatite. Thus, these findings seem promising for developing innovative Nb-doped calcium phosphates as artificial biomaterials for potential use in bone replacements and repair.

Preparation, characterization of Mo catalysts supported on Ni- containing calcium deficient hydroxyapatite and reactivity for the thiophene HDS reaction

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Cherif A.

2013-09-01

Full Text Available Ni-containing Calcium Hydroxyapatite (NiCaHAp; 3.31 wt.% Ni was synthesized by coprecipitation and used as catalyst support. Molybdenum was supported on NiCaHAp by impregnation using ammonium heptamolybdate. The prepared catalysts Mo(x/NiCaHAp (x: 2 to 8 wt % in Mo were characterized by elemental analysis, XRD, FT-IR, N2 adsorption-desorption and TEM-EDX. The catalysts were sulfided in-situ at 673 K under flowing H2S/H2 (15 Vol.% H2S and tested in hydrodesulfurization (HDS of thiophene at 673 K. The main XRD peaks of hydroxyapatite CaHAp phase were observed in all samples and a peak due probably to crystalline MoO3 phase was also identified from the results. However, no crystalline phase of NiO was found for the catalysts, which showed its Ni species were highly dispersed. The sulfided catalysts Mo(x/NiCaHAp presented are active in HDS of thiophene, despite the presence of some large MoO3 crystallites and incomplete sulfidation. This activity may be due to interaction of NiO and MoO3 on CaHAp resulting in the formation of Ni-Mo-S phase under flowing H2S/H2. When the molybdenum content increased the HDS activity increasead slightly, which was caused by the agglomeration of MoO3. The Mo(8/NiCaHAp catalyst is about two times less active for thiophene HDS than the commercial NiMoP/Al2O3.

The effect of polymerization mode on monomer conversion, free radical entrapment, and interaction with hydroxyapatite of commercial self-adhesive cements.

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D'Alpino, Paulo Henrique Perlatti; Silva, Marília Santos; Vismara, Marcus Vinícius Gonçalves; Di Hipólito, Vinicius; Miranda González, Alejandra Hortencia; de Oliveira Graeff, Carlos Frederico

2015-06-01

This study evaluated the degree of conversion, the free radical entrapment, and the chemical interaction of self-adhesive resin cements mixed with pure hydroxyapatite, as a function of the polymerization activation mode among a variety of commercial self-adhesive cements. Four cements (Embrace WetBond, MaxCem Elite, Bifix SE, and RelyX U200) were mixed, combined with hydroxyapatite, dispensed into molds, and distributed into three groups, according to polymerization protocols: IP (photoactivation for 40s); DP (delayed photoactivation, 10 min self-curing plus 40s light-activated); and CA (chemical activation, no light exposure). Infrared (IR) spectra were obtained and monomer conversion (%) was calculated by comparing the aliphatic-to-aromatic IR absorption peak ratio before and after polymerization (n=10). The free radical entrapment values of the resin cements were characterized using Electron Paramagnetic Resonance (EPR) and the concentration of spins (number of spins/mass) calculated (n=3). Values were compared using two-way ANOVA and Tukey's post-hoc test (α=5%). X-ray diffraction (XRD) characterized the crystallinity of hydroxyapatite as a function of the chemical interactions with the resin cements. The tested parameters varied as a function of resin cement and polymerization protocol. Embrace WetBond and RelyX U200 demonstrated dependence on photoactivation (immediate or delayed), whereas MaxCem Elite exhibited dependence on the chemical activation mode. Bifix SE presented the best balance based on the parameters analyzed, irrespective of the activation protocol. Choice of polymerization protocol affects the degree of conversion, free radical entrapment, and the chemical interaction between hydroxyapatite and self-adhesive resin cement mixtures. Copyright © 2015 Elsevier Ltd. All rights reserved.

Characterization of hydroxyapatite substituted with silicon

International Nuclear Information System (INIS)

Silva, H.M. da; Soares, G.A.; Mateescu, M.; Anselme, K.; Palard, M.; Champion, E.

2009-01-01

Incorporation of silicon (Si) ions into hydroxyapatite structure (HA) influences on physical, chemical and physiological properties. Some studies reported the improved bioactivity Si substitution, and it also accelerates the biomineralization process. The main objective of this work is to characterize stoichiometric hydroxyapatite and hydroxyapatite substituted with 1.13% in weight of Si (SiHA) using a wet precipitation method followed by a heat treatment. SEM/EDS, AFM, DRX and FTIR analyses were used to characterize the samples. EDS and FTIR results confirmed the presence of Si. Silicon induces small changes on crystal structure of HA, not detected on X-ray diffraction patterns of sintered tablets of SiHA and HA. No secondary phases were observed, that indicates the Si had entered the HA lattice. (author)

Si-substituted hydroxyapatite nanopowders: Synthesis, thermal stability and sinterability

International Nuclear Information System (INIS)

Bianco, Alessandra; Cacciotti, Ilaria; Lombardi, Mariangela; Montanaro, Laura

2009-01-01

Synthetic hydroxyapatites incorporating small amounts of Si have shown improved biological performances in terms of enhanced bone apposition, bone in-growth and cell-mediated degradation. This paper reports a systematic investigation on Si-substituted hydroxyapatite (Si 1.40 wt%) nanopowders produced following two different conventional wet methodologies: (a) precipitation of Ca(NO 3 ) 2 .4H 2 O and (b) titration of Ca(OH) 2 . The influence of the synthesis process on composition, thermal behaviour and sinterability of the resulting nanopowders is studied. Samples were characterised by electron microscopy, induced coupled plasma atomic emission spectroscopy, thermal analysis, infrared spectroscopy, N 2 adsorption measurements, X-ray diffraction and dilatometry. Semicrystalline Si-substituted hydroxyapatite powders made up of needle-like nanoparticles were obtained, the specific surface area ranged between 84 and 110 m 2 /g. Pure and Si-substituted hydroxyapatite nanopowders derived from Ca(NO 3 ) 2 .4H 2 O decomposed around 1000 deg. C. Si-substituted hydroxyapatite nanopowders obtained from Ca(OH) 2 were thermally stable up to 1200 deg. C and showed a distinct decreased thermal stability with respect to the homologous pure sample. Si-substituted hydroxyapatites exhibited higher sintering temperature and increased total shrinkage with respect to pure powders. Nanostructured dense ceramics were obtained by sintering at 1100 deg. C Si-substituted hydroxyapatites derived from Ca(OH) 2

The synthesis of hydroxyapatite through the precipitation method

International Nuclear Information System (INIS)

Shah Rizal, K.; Fahmi, M.N.; Mat Akil, H.; Zainal Arifin, A.

2004-01-01

Hydroxyapatite (HA) has been earmarked as suitable for implantation within the human body due to the similarity of its chemical makeup to human bone, In this paper, HA powders were synthesized via the precipitation method where phosphoric acid (H 3 PO 4 ) was titrated into calcium hydroxide solution [Ca(OH) 2 ]. Two parameters such as temperature and stirring rate were identified as factors that influenced the amount and purity of HA powder, Phase identification of the synthesized powder was done using X-Ray Diffraction (XRD). The results show that HA phase can be synthesized from this titration process of Ca(OH) 2 and H 3 PO 4 with yield amount of HA powder around 45-61 grams but with less than hundred percent purity. In order to study the effect of heat treatment to RA crystals structure, HA powder was calcined at 850 degree C for 2 hours. Its found that the degree of crystallinity increases after calcination because of lattice expansion when the materials were heated at higher temperature. (Author)

Effect of a calcium cathode on water-based nanoparticulate solar cells

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Vaughan, Ben; Stapleton, Andrew; Xue, Bofei; Sesa, Elisa; Zhou, Xiaojing; Bryant, Glenn; Belcher, Warwick; Dastoor, Paul

2012-07-01

Water-based nanoparticulate (NP) and bulk heterojunction (BHJ) organic photovoltaic (OPV) devices based on blends of poly(9,9-dioctylfluorene-co-N,N-bis(4-butylphenyl)-N,Ndiphenyl-1,4-phenylenediamine) (PFB) and poly(9,9-dioctylfluorene-co-benzothiadiazole (F8BT) have been fabricated with aluminium and calcium/aluminium cathodes. The NP devices exhibit power conversion efficiencies (PCEs) that are double that of the corresponding BHJ device. Moreover, the addition of calcium into the cathode structure results in a dramatic increase in open circuit voltage and PCEs approaching 1% for water-based polyfluorene OPV devices.

Characteristics of porous zirconia coated with hydroxyapatite

Indian Academy of Sciences (India)

However, porous hydroxyapatite bodies are mechanically weak and brittle, which makes shaping and implantation difficult. One way to solve this problem is to introduce a strong porous network onto which hydroxyapatite coating is applied. In this study, porous zirconia and alumina-added zirconia ceramics were prepared ...

Hydroxyapatite nanorods: soft-template synthesis, characterization and preliminary in vitro tests.

Science.gov (United States)

Nguyen, Nga Kim; Leoni, Matteo; Maniglio, Devid; Migliaresi, Claudio

2013-07-01

Synthetic hydroxyapatite nanorods are excellent candidates for bone tissue engineering applications. In this study, hydroxyapatite nanorods resembling bone minerals were produced by using soft-template method with cetyltrimethylammonium bromide. Composite hydroxyapatite/poly(D, L)lactic acid films were prepared to evaluate the prepared hydroxyapatite nanorods in terms of cell affinity. Preliminary in vitro experiments showed that aspect ratio and film surface roughness play a vital role in controlling adhesion and proliferation of human osteoblast cell line MG 63. The hydroxyapatite nanorods with aspect ratios in the range of 5.94-7 were found to possess distinctive properties, with the corresponding hydroxyapatite/poly(D, L)lactic acid films promoting cellular confluence and a fast formation of collagen fibers as early as after 7 days of culture.

An improved biofunction of titanium for keratoprosthesis by hydroxyapatite-coating.

Science.gov (United States)

Dong, Ying; Yang, Jingxin; Wang, Liqiang; Ma, Xiao; Huang, Yifei; Qiu, Zhiye; Cui, Fuzhai

2014-03-01

Titanium framework keratoprosthesis has been commonly used in the severe corneal blindness, but the tissue melting occurred frequently around titanium. Since hydroxyapatite has been approved to possess a good tissue integration characteristic, nanostructured hydroxyapatite was coated on the surface of titanium through the aerosol deposition method. In this study, nanostructured hydroxyapatite coating was characterized by X-ray diffraction, scanning electron microscopy, atomic force microscopy, and auger electronic spectrometer. Biological evaluations were performed with rabbit cornea fibroblast in vitro and an animal model in vivo. The outcomes showed the coating had a grain-like surface topography and a good atomic mixed area with substrate. The rabbit cornea fibroblasts appeared a good adhesion on the surface of nanostructured hydroxyapatite in vitro. In the animal model, nanostructured hydroxyapatite-titanium implants were stably retained in the rabbit cornea, and by contrast, the corneal stroma became thinner anterior to the implants in the control. Therefore, our findings proved that nanostructured hydroxyapatite-titanium could not only provide an improved bond for substrate but also enhance the tissue integration with implants in host. As a promising material, nanostructured hydroxyapatite-titanium-based keratoprosthesis prepared by the aerosol deposition method could be utilized for the corneal blindness treatment.

Synthesis of hydroxyapatite nanoparticles from egg shells by sol-gel method

Science.gov (United States)

Azis, Y.; Adrian, M.; Alfarisi, C. D.; Khairat; Sri, R. M.

2018-04-01

Hydroxyapatite, [Ca10(PO4)6(OH)2, (HAp)] is widely used in medical fields especially as a bone and teeth substitute. Hydroxyapatite nanoparticles have been succesfully synthesized from egg shells as a source of calcium by using sol-gel method. The egg shells were calcined, hydrated (slaking) and undergone carbonation to form Precipitated Calcium Carbonate (PCC).Then the PCC was added (NH4)2HPO4 to form HAp with variation the mole ratio Ca and P (1.57; 1.67 and 1.77), aging time (24, 48, and 72 hr) and under basic condition pH (9, 10 and 11). The formation of hydroxyapatite biomaterial was characterized using XRD, FTIR, SEM-EDX. The XRD patterns showed that the products were hydroxyapatite crystals. The best result was obtained at 24 hr aging time, pH 9 with hexagonal structure of hydroxyapatite. Particle size of HAp was 35-54 nm and the morphology of hydroxyapatite observed using SEM, it showed that the uniformity crystal of hydroxyapatite.

Nano-particulate Aluminium Nitride/Al: An Efficient and Versatile Heterogeneous Catalyst for the Synthesis of Biginelli Scaffolds

Science.gov (United States)

Tekale, S. U.; Tekale, A. B.; Kanhe, N. S.; Bhoraskar, S. V.; Pawar, R. P.

2011-12-01

Nano-particulate aluminium nitride/Al (7:1) is reported as a new heterogeneous solid acid catalyst for the synthesis of 3, 4-dihydroxypyrimidi-2-(1H)-ones and their sulphur analogues using the Biginelli reaction. This method involves short reaction time, easy separation, high yields and purity of products.

Microstructural characteristics of the hydroxyapatite and its influence in the Tl signal induced by gamma radiation

International Nuclear Information System (INIS)

Mendoza A, D.; Gonzalez M, P.R.; Hernandez A, M.; Estrada G, R.; Rodriguez L, V.

2003-01-01

The analysis carried out on different materials has shown that the quantity and type of dopants play an important role in the behaviour thermoluminescent signal induced by the ionizing radiation. More recent studies have also shown that the grain size influences strongly in the thermoluminescent signal. Plus still, the crystal growth habit and the crystalline degree have an important effect in the type and intensity thermoluminescent signal. In this sense, we present this work on the analysis of the thermoluminescent signal induced by the gamma radiation in the hydroxyapatite ceramic. Depending the growth habit, a variation of the peak temperature location, signal intensity and linearity range was observed; in particular cases a lineal relationship between glow curve and radiation dose was in the range from 2 to 1000 Gray. These results are complemented with a microstructural and crystalline degree analysis through scanning electron microscopy and X-ray Diffraction. The dose-response over the whole irradiation range opening up the possibility of employing this bio material as a dosimeter. (Author)

Hydroxyapatites and europium(III) doped hydroxyapatites as a carrier of silver nanoparticles and their antimicrobial activity.

Science.gov (United States)

Wiglusz, Rafal J; Kedziora, Anna; Lukowiak, Anna; Doroszkiewicz, Wlodzimierz; Strek, Wieslaw

2012-08-01

Hydroxyapatites (Ca10(PO4)6(OH)2 and Eu3+:Ca10(PO4)6(OH)2) were synthesized by aqueous synthesis route. Hydroxyapatites were impregnated with silver ions that were subsequently reduced. XRD, TEM, and SAED measurements were used in order to determine the crystal structure and morphology of the final products. The results showed the well crystallized hydroxyapatite grains with diameter of about 35 nm and with silver nanoparticles on their surface. The antimicrobial activity of the nanoparticles against: Staphylococcus aureus ATCC 6538 as model of the Gram-positive bacteria, Escherichia coli ATCC 11229, and Klebsiella pneumoniae ATCC 4352 as model of Gram-negative bacteria, were shown with the best activity against K. pneumoniae. These nanocomposite powders can be a promising antimicrobial agent and a fluorescent material for biodetection due to their optical and bioactive properties.

Neuropathic Pain and Lung Delivery of Nanoparticulate Drugs: An Emerging Novel Therapeutic Strategy.

Science.gov (United States)

Islam, Nazrul; Abbas, Muzaffar; Rahman, Shafiqur

2017-01-01

Neuropathic pain is a chronic neurological disorder affecting millions of people around the world. The currently available pharmacologic agents for the treatment of neuropathic pain have limited efficacy and are associated with dose related unwanted adverse effects. Due to the limited access of drug molecules across blood-brain barrier, a small percentage of drug that is administered systematically, reaches the central nervous system in active form. These therapeutic agents also require daily treatment regimen that is inconvenient and potentially impact patient compliance. Application of nanoparticulate drugs for enhanced delivery system has been explored extensively in the last decades. Pulmonary delivery of nanomedicines for the management of various diseases has become an emerging treatment strategy that ensures the targeted delivery of drugs both for systemic and local effects with low dose and limited adverse effects. To the best of our knowledge, there are no inhaled drug products available on market for the treatment of neuropathic pain. The advantages of delivering therapeutics into deep lungs include non-invasive drug delivery, higher bioavailability with low dose, lower systemic toxicity, and potentially greater blood-brain barrier penetration. This review discusses and highlights the important issues on the application of emerging nanoparticulate lung delivery of drugs for the effective treatment of neuropathic pain. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

In situ growth of hydroxyapatite within electrospun poly(DL-lactide) fibers.

Science.gov (United States)

Cui, Wenguo; Li, Xiaohong; Zhou, Shaobing; Weng, Jie

2007-09-15

Development of nanocomposites of hydroxyapatite (HA) and polylactic acid (PLA) is attractive, as the advantageous properties of the two types of materials can be combined to suit better the mechanical and biological demands for biomedical uses. To solve the problematic issue of agglomeration of HA crystallites in the PLA matrix, a novel method is introduced in the present study to use electrospun nanofibers as the reaction confinement for composite fabrication. Poly(DL-lactide) ultrafine fibers with calcium nitrate entrapment were prepared by electrospinning and then incubated in phosphate solution to form in situ calcium phosphate on the polymer matrix. The formation of nonstoichiometric nanostructured HA and well dispersion of HA particles on the electrospun fibers were observed. Higher crystalline HA phase was indicated in samples after sintering at 1200 degrees C. The formation of the calcium-phosphate phase was dependent upon the precipitation conditions, and the effects of the incubation time, temperature, and the pH values of the incubation medium were investigated on the spontaneous precipitation and amorphous-crystalline transformation of HA in the current study. Considering the biodegradability of matrix polymer and the crystallinity and uniform dispersal of HA, optimal conditions for composite preparation were incubating calcium-containing ultrafine fibers at 37 degrees C in pH 7.4 or at 25 degrees C in pH 9.0 of diammonium hydrogen phosphate solutions for 7 days. Around 25%-34% of mineral contents can be synthesized in the resulting composites, which was higher than the theoretical value due to the nonstoichiometric HA formed in the composite, and the fiber degradation and partial calcium nitrate involved in the HA formation. Copyright 2007 Wiley Periodicals, Inc.

Fine structure study on low concentration zinc substituted hydroxyapatite nanoparticles

International Nuclear Information System (INIS)

Hu, Wei; Ma, Jun; Wang, Jianglin; Zhang, Shengmin

2012-01-01

The fine structure of zinc substituted hydroxyapatite was studied using experimental analysis and first-principles calculations. The synthetic hydroxyapatite nanoparticles containing low Zn concentration show rod-like morphology. The crystallite sizes and unit-cell volumes tended to decrease with the increased Zn concentration according to X-ray diffraction patterns. The Zn K-edge X-ray absorption spectra and fitting results suggest that the hydroxyapatite doped with 0.1 mole% zinc is different in the zinc coordination environments compared with that containing more zinc. The density function theory calculations were performed on zinc substituted hydroxyapatite. Two mechanisms included replacing calcium by zinc and inserting zinc along the hydroxyl column and were investigated, and the related substitution energies were calculated separately. It is found that the substitution energies are negative and lowest for inserting zinc between the two oxygen atoms along the hydroxyl column (c-axis). Combined with the spectral analysis, it is suggested that the inserting mechanism is favored for low concentration zinc substituted hydroxyapatite. Highlights: ► We investigate the fine structure of hydroxyapatite with low content of Zn. ► XANES spectra are similar but a little different at low zinc content. ► Zinc ions influence hydroxyapatite crystal formation and lattice parameters. ► Formation energies are calculated according to plane-wave density function theory. ► Low content of zinc prefers to locate at hydroxyl column in hydroxyapatite lattice.

Development of lattice-inserted 5-Fluorouracil-hydroxyapatite nanoparticles as a chemotherapeutic delivery system.

Science.gov (United States)

Tseng, Ching-Li; Chen, Jung-Chih; Wu, Yu-Chun; Fang, Hsu-Wei; Lin, Feng-Huei; Tang, Tzu-Piao

2015-10-01

Developing an effective vehicle for cancer treatment, hydroxyapatite nanoparticles were fabricated for drug delivery. When 5-Fluorouracil, a major chemoagent, is combined with hydroxyapatite nanocarriers by interclay insertion, the modified hydroxyapatite nanoparticles have superior lysosomal degradation profiles, which could be leveraged as controlled drug release. The decomposition of the hydroxyapatite nanocarriers facilitates the release of 5-Fluorouracil into the cytoplasm causing cell death. Hydroxyapatite nanoparticles with/without 5-Fluorouracil were synthesized and analyzed in this study. Their crystallization properties and chemical composition were examined by X-ray diffraction and Fourier transforms infrared spectroscopy. The 5-Fluorouracil release rate was determined by UV spectroscopy. The biocompatibility of hydroxyapatite-5-Fluorouracil extraction solution was assessed using 3T3 cells via a WST-8 assay. The effect of hydroxyapatite-5-Fluorouracil particles which directly work on the human lung adenocarcinoma (A549) cells was evaluated by a lactate dehydrogenase assay via contact cultivation. A 5-Fluorouracil-absorbed hydroxyapatite particles were also tested. Overall, hydroxyapatite-5-Fluorouracils were prepared using a co-precipitation method wherein 5-Fluorouracil was intercalated in the hydroxyapatite lattice as determined by X-ray diffraction. Energy dispersive scanning examination showed the 5-Fluorouracil content was higher in hydroxyapatite-5-Fluorouracil than in a prepared absorption formulation. With 5-Fluorouracil insertion in the lattice, the widths of the a and c axial constants of the hydroxyapatite crystal increased. The extraction solution of hydroxyapatite-5-Fluorouracil was nontoxic to 3T3 cells, in which 5-Fluorouracil was not released in a neutral phosphate buffer solution. In contrast, at a lower pH value (2.5), 5-Fluorouracil was released by the acidic decomposition of hydroxyapatite. Finally, the results of the lactate

Nanosized Hydroxyapatite Precipitation on the Ti—30Ta—xHf Alloys.

Science.gov (United States)

Lee, Kang; Jang, Jae- In; Han-Cheol, Choe

2017-04-01

In this study, we prepared hydroxyapatite (HAp) layer on the alkali treated Ti–30Ta–xHf alloys using electrochemical deposition method. Ti–30Ta–xHf alloys was anodized in 5 M NaOH solution at 0.3 A for 10 min. Alkali treated Ti–30Ta–xHf surface formed by anodization step which acted as templates and anchorage for growth of the HAp during subsequent pulsed electrochemical deposition process at 85 °C. The phase and morphologies of deposited HAp layer were affected by the Hf contents of Ti–30Ta–xHf alloys. The nano-scale rod-like HAp layer was formed on untreated Ti–30Ta–xHf alloys with partially low crystallinity. In the case of alkali treated Ti–30Ta–xHf, nano-sized needle-like layers were transferred to nano-flake surface and denser morphology as Hf content increased.

Simple synthetic route for hydroxyapatite colloidal nanoparticles via a Nd:YAG laser ablation in liquid medium

Science.gov (United States)

Mhin, Sung Wook; Ryu, Jeong Ho; Kim, Kang Min; Park, Gyeong Seon; Ryu, Han Wool; Shim, Kwang Bo; Sasaki, Takeshi; Koshizaki, Naoto

2009-08-01

Pulsed laser ablation (PLA) in liquid medium was successfully employed to synthesize hydroxyapatite (HAp) colloidal nanoparticles. The crystalline phase, particle morphology, size distribution and microstructure of the HAp nanoparticles were investigated in detail. The obtained HAp nanoparticles had spherical shape with sizes ranging from 5 to 20 nm. The laser ablation and the nanoparticle forming process were studied in terms of the explosive ejection mechanism by investigating the change of the surface morphology on target. The stoichiometry and bonding properties were studied by using XPS, FT-IR and Raman spectroscopy. A molar ratio of Ca/P of the prepared HAp nanoparticles was more stoichiometric than the value reported in the case of ablation in vacuum.

The Influence of Carbonate Ions on the Structure of the Electrical Double Layer at the Interface of Hydroxyapatite/Electrolyte Solution

Directory of Open Access Journals (Sweden)

Ewa SKWAREK

2016-05-01

Full Text Available The aim of the work was to investigate the changes in the double electrical layer at the hydroxyapatite containing different amount of carbonate ions/electrolyte solution. Besides, the main properties of the edl (electrical double layer, i.e. surface charge density and zeta potential were determined by electrophoresis measurements and potentiometer titration, respectively. The synthesized adsorbents were characterized by the following methods: X-ray diffraction, FTIR (Fourier Transform Infrared Spectroscopy, adsorption and desorption of nitrogen and scanning electron microscopy. The analyzed samples had different structures and particle sizes. It was proved that increase in the carbonate groups content is connected with the decrease of apatite grain sizes and crystallinity reduction. The characteristic parameters of the electric double layer were also different: pHpzc (point zero of charge of hydroxyapatite was 6.5 whereas for carbonate apatite was higher – pHpzc = 8. In both cases determination of precise pHIEP (isoelectric point was not possible but it is known that its value is lower than 4.DOI: http://dx.doi.org/10.5755/j01.ms.22.2.7817

Fabrication, ultra-structure characterization and in vitro studies of RF magnetron sputter deposited nano-hydroxyapatite thin films for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Surmeneva, Maria A. [Department of Theoretical and Experimental Physics, National Research Tomsk Polytechnic University, Tomsk 634050 (Russian Federation); Surmenev, Roman A., E-mail: rsurmenev@gmail.com [Department of Theoretical and Experimental Physics, National Research Tomsk Polytechnic University, Tomsk 634050 (Russian Federation); Fraunhofer Institute for Interfacial Engineering and Biotechnology IGB, 70569 Stuttgart (Germany); Nikonova, Yulia A.; Selezneva, Irina I. [Institute of Theoretical and Experimental Biophysics, Russian Academy of Sciences, Pushchino 142292 (Russian Federation); Ivanova, Anna A. [Department of Theoretical and Experimental Physics, National Research Tomsk Polytechnic University, Tomsk 634050 (Russian Federation); Putlyaev, Valery I. [Department of Chemistry, Moscow State University, Vorobievi Gory, 1, Moscow 119991 (Russian Federation); Prymak, Oleg; Epple, Matthias [Inorganic Chemistry and Center for Nanointegration Duisburg-Essen (CeNIDE), University of Duisburg-Essen, 45117 Essen (Germany)

2014-10-30

Highlights: • Growth of a columnar grain structure perpendicular to the substrate surface was observed. • Interplanar spacing distances measured using HRTEM were 0.82 and 0.28 nm, corresponding to the (0 0 1) and (2 1 1) lattice planes of hexagonal HA. • Grain size and crystallinity increased when increasing the deposition time. • Nanometer-thick low-crystallinity HA coatings with different thicknesses stimulated cells to attach, proliferate and form mineralized nodules. - Abstract: A series of nanostructured low-crystalline hydroxyapatite (HA) coatings averaging 170, 250, and 440 nm in thickness were deposited onto previously etched titanium substrates through radio-frequency (RF) magnetron sputtering. The HA coatings were analyzed using infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM). Cross sections of the thin specimens were prepared by FIB to study the microstructure of the coatings by TEM. The deposition process formed nano-scale grains, generating an amorphous layer at the substrate/coating interface and inducing the growth of a columnar grain structure perpendicular to the substrate surface. A microstructural analysis of the film confirmed that the grain size and crystallinity increased when increasing the deposition time. The nanostructured HA coatings were not cytotoxic, as proven by in vitro assays using primary dental pulp stem cells and mouse fibroblast NCTC clone L929 cells. Low-crystallinity HA coatings with different thicknesses stimulated cells to attach, proliferate and form mineralized nodules on the surface better than uncoated titanium substrates.

The hydroxyapatite-binding regions of a rat salivary glycoprotein.

Science.gov (United States)

Embery, G; Green, D R

1989-09-01

The regions of a salivary sulphated glycoprotein which are involved in its attachment to hydroxyapatite (Biogel HTP) have been characterised. The sulphated glycoprotein, a 35S-labelled preparation from mixed palatal and buccal minor gland secretions of the rat was bound onto hydroxyapatite and the resultant glycoprotein-hydroxyapatite complex was sequentially digested with pronase E and alpha-L-fucosidase, a treatment which released 86.8% +/- 1.7% of the radioactivity of the initially bound glycoprotein. The fragments which remained attached to the hydroxyapatite after enzymic digestion were fractionated on Sephadex G-25 and analysed for carbohydrate and amino acid components. A range of amino acids were detected which could reflect both glycosylated and non-glycosylated-binding regions. Sialic acid, although considered to be involved in the attachment process was not detected in any of the fragments remaining after enzymic digestion, a finding which provides indirect evidence that the enzymically liberated products do not subsequently re-attach to the hydroxyapatite surface. The notable feature of the fractions with average Mr estimated at 1000 or less is the high proportion of N-acetylhexosamine and N-acetylgalactosamine. It is apparent that the hexosamine residues, which normally bear the ester sulphate moieties of sulphated glycoproteins, play an important role in the attachment of sulphated glycoproteins to hydroxyapatite.

Characterization and inhibitive study of gel-grown hydroxyapatite crystals at physiological temperature

Science.gov (United States)

Parekh, Bharat; Joshi, Mihir; Vaidya, Ashok

2008-04-01

Hydroxyapatite is very useful for various biomedical applications, due to its chemical similarity with mineralized bone of human. Hydroxyapatite is also responsible for arthropathy (joint disease). In the present study, the growth of hydroxyapatite crystals was carried out by using single-diffusion gel growth technique in silica hydro gel media, at physiological temperature. The growth of hydroxyapatite crystals under slow and controlled environment in gel medium can be simulated in a simple manner to the growth in human body. The crystals, formed in the Liesegang rings, were characterized by powder XRD, FTIR and dielectric study. The diffusion study is also carried out for the hydroxyapatite crystals using the moving boundary model. The inhibitive influence of various Ayurvedic medicinal plant extracts such as Boswellia serrata gum resin , Tribulus terrestris fruits, Rotula aquatica roots, Boerhaavia diffusa roots and Commiphora wightii, on the growth of hydroxyapatite was studied. Roots of R. aquatica and B. diffusa show some inhibition of the hydroxyapatite crystals in vitro. This preclinical study will be helpful to design the therapy for prevention of hydroxyapatite-based ailments.

Improvement of the stability of hydroxyapatite through glass ceramic reinforcement.

Science.gov (United States)

Ha, Na Ra; Yang, Zheng Xun; Hwang, Kyu Hong; Kim, Tae Suk; Lee, Jong Kook

2010-05-01

Hydroxyapatite has achieved significant application in orthopedic and dental implants due to its excellent biocompatibility. Sintered hydroxyapatites showed significant dissolution, however, after their immersion in water or simulated body fluid (SBF). This grain boundary dissolution, even in pure hydroxyapatites, resulted in grain separation at the surfaces, and finally, in fracture. In this study, hydroxyapatite ceramics containing apatite-wollastonite (AW) or calcium silicate (SG) glass ceramics as additives were prepared to prevent the dissolution. AW and SG glass ceramics were added at 0-7 wt% and powder-compacted uniaxially followed by firing at moisture conditions. The glass phase was incorporated into the hydroxyapatite to act as a sintering aid, followed by crystallization, to improve the mechanical properties without reducing the biocompatibility. As seen in the results of the dissolution test, a significant amount of damage was reduced even after more than 14 days. TEM and SEM showed no decomposition of HA to the secondary phase, and the fracture toughness increased, becoming even higher than that of the commercial hydroxyapatite.

Microwave assisted synthesis of hydroxyapatite nano strips

Energy Technology Data Exchange (ETDEWEB)

Ruban Kumar, A.; Kalainathan, S.; Saral, A.M. [School of Advanced Sciences, VIT University, Vellore 632014, Tamil Nadu (India)

2010-07-15

Synthesis of hydroxyapatite (HAP) nano strips was carried out by chemical precipitation method followed by microwave irradiation. The microwave assisted reactions proceed at fast rates. It is found that the presence of the complex reagent EDTA plays an important role in the morphological changes of nanostructure hydroxyapatite. EDTA acts as a hexadentate unit by wrapping itself around the Ca{sup 2+} metal ion with, four oxygen and two nitrogen atoms and forms several five member chelate rings. The relative specific surface energies associated with the facets of the crystal determines the shape of the crystal. Scanning electron microscopy revealed the presence of hydroxyapatite nano strips with the range 50-100 nm in EDTA influenced HAP powders. Fourier transform-infrared spectroscopy (FT-IR) result combined with the X-ray diffraction (XRD) indicates the presence of amorphous hydroxyapatite (HAP) in the as-prepared material. X-ray patterns collected on the powder after heat-treatment at 1100 C for 2 h in air exhibits single phase of HAP. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Protein Adsorption and Antibacterial Behavior for Hydroxyapatite Nanocrystals Prepared by Hydrothermal Method

OpenAIRE

笠原, 英充; 小形, 信男; 荻原, 隆

2005-01-01

Homogeneous hydroxyapatite nanocrystals which have aspect ratio with more than four were synthesized by hydrothermal method. X-ray fluorescence analysis revealed that the Ca/P ratio of hydroxyapatite nanocrystals was maintaining start composition. The protein adsorption properties and bacteria-resistant of hydroxyapatite nanocrystals were investigated. The protein adsorption properties of hydroxyapatite nanocrystals were improvement after the hydrothermal treatment. Bacteria-resistant behavio...

Thermal and ultrasonic influence in the formation of nanometer scale hydroxyapatite bio-ceramic

Science.gov (United States)

Poinern, GJE; Brundavanam, R; Le, X Thi; Djordjevic, S; Prokic, M; Fawcett, D

2011-01-01

Hydroxyapatite (HAP) is a widely used biocompatible ceramic in many biomedical applications and devices. Currently nanometer-scale forms of HAP are being intensely investigated due to their close similarity to the inorganic mineral component of the natural bone matrix. In this study nano-HAP was prepared via a wet precipitation method using Ca(NO3)2 and KH2PO4 as the main reactants and NH4OH as the precipitator under ultrasonic irradiation. The Ca/P ratio was set at 1.67 and the pH was maintained at 9 during the synthesis process. The influence of the thermal treatment was investigated by using two thermal treatment processes to produce ultrafine nano-HAP powders. In the first heat treatment, a conventional radiant tube furnace was used to produce nano-particles with an average size of approximately 30 nm in diameter, while the second thermal treatment used a microwave-based technique to produce particles with an average diameter of 36 nm. The crystalline structure and morphology of all nanoparticle powders produced were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR). Both thermal techniques effectively produced ultrafine powders with similar crystalline structure, morphology and particle sizes. PMID:22114473

Development of hydroxyapatite bone cement for controlled drug ...

Indian Academy of Sciences (India)

The purpose of this work was to study the preparation and characterization of drug–hydroxyapatite cement. The hydroxyapatite (HA) cement has been synthesized by using tricalcium phosphate, calcium carbonate and dicalcium phosphate anhydrous with sodium hydrogen phosphate as liquid phase. The effect of added ...

Sorption of zinc on synthetic hydroxyapatite from aqueous solution

International Nuclear Information System (INIS)

Pivarciova, L.; Rosskopfova, O.; Galambos, M.; Rajec, P.

2014-01-01

The sorption of Zn 2+ on synthetic hydroxyapatite was investigated using a batch method and radiotracer technique. This work was aimed to study influence of the contact time, effect of pH and different concentration of Zn 2+ ions in the solution. The percentage of zinc adsorption on HA1 and HA2 was more than 96 % during 1 h for initial Zn 2+ concentration of 1·10 -4 .5·10 -4 and 1·10 -3 mol·dm -3 . The equilibrium time of 2 h was chosen for further experiments. The sorption of zinc on hydroxyapatite was pH independent ranging from 4.5 to 6.5 as a result of buffering properties of hydroxyapatite. The experimental data for adsorption of zinc have been interpreted in the term of Langmuir isotherm and the value of maximum adsorption capacity of zinc on a commercial hydroxyapatite and hydroxyapatite prepared by wet precipitation process was calculated to be 0.437 mmol·g -1 and 0.605 mmol·g -1 , respectively. (authors)

Adsorption mechanism of BMP-7 on hydroxyapatite (001) surfaces

International Nuclear Information System (INIS)

Zhou, Hailong; Wu, Tao; Dong, Xiuli; Wang, Qi; Shen, Jiawei

2007-01-01

Many properties and functions of bone-related proteins perform through the interface with the hydroxyapatite. However, the mechanism of difference of proteins adsorbing behaviors caused by the variation of calcium and phosphate ions on hydroxyapatite is still unclear at atomic level. In this work, we investigated the site-selective adhesion and the adsorption mechanism of protein BMP-7 to the hydroxyapatite surfaces in aqueous media during adsorption and desorption processes. Molecular dynamics (MD) and steered molecular dynamics (SMD) simulations combined with trajectory analysis were employed to give insight into the underlying behaviors of BMP-7 binding. The results suggest that the adsorption sites could be divided into two categories: COO - and NH 2 /NH3+. For COO - , the adsorption phenomenon is driven by the electrostatic interaction formed between the negative charged carboxylate groups and the Ca1 cations on the hydroxyapatite surface. While for NH 2 /NH3+, the interaction is through the intermolecular H-bonds between the N-containing groups and the phosphate on the hydroxyapatite surface

[In Situ Polymerization and Characterization of Hydroxyapatite/polyurethane Implanted Material].

Science.gov (United States)

Gu, Muqing; Xiao, Fengjuan; Liang, Ye; Yue, Lin; Li, Song; Li, Lanlan; Feng, Feifei

2015-08-01

In order to improve the interfacial bonding strength of hydroxyapatite/polyurethane implanted material and dispersion of hydroxyapatite in the polyurethane matrix, we in the present study synthesized nano-hydroxyapatite/polyurethane composites by in situ polymerization. We then characterized and analyzed the fracture morphology, thermal stability, glass transition temperature and mechanical properties. We seeded MG63 cells on composites to evaluate the cytocompatibility of the composites. In situ polymerization could improve the interfacial bonding strength, ameliorate dispersion of hydroxyapatite in the properties of the composites. After adding 20 wt% hydroxyapatite into the polyurethane, the thermal stability was improved and the glass transition temperatures were increased. The tensile strength and maximum elongation were 6.83 MPa and 861.17%, respectively. Compared with those of pure polyurethane the tensile strength and maximum elongation increased by 236.45% and 143.30%, respectively. The composites were helpful for cell adhesion and proliferation in cultivation.

Hydroxyapatite coatings on titanium dioxide thin films prepared by pulsed laser deposition method

International Nuclear Information System (INIS)

Suda, Yoshiaki; Kawasaki, Hiroharu; Ohshima, Tamiko; Nakashima, Shouta; Kawazoe, Syuichi; Toma, Tetsuya

2006-01-01

Hydroxyapatite (HAp) coated on titanium dioxide (TiO 2 ) thin films has been developed to supplement the defects of both TiO 2 and HAp. Thin films have been prepared by pulsed laser deposition (PLD) method using HAp and HAp(10%) + TiO 2 targets. X-ray diffraction (XRD) shows that there are many small peaks of Ca 1 0(PO 4 ) 6 (OH) 2 crystal, and no impurity other than HAp is detected in HAp films prepared using pure HAp target. The composition ratio of the film was analyzed by X-ray photoelectron spectroscopy (XPS). HAp coatings on TiO 2 thin films have been prepared using HAp(10%) + TiO 2 targets. XRD and XPS measurements suggest that crystalline HAp + TiO 2 thin films are obtained by the PLD method using HAp(10%) + TiO 2 target

Identification of glycosaminoglycans using high-performance liquid chromatography on a hydroxyapatite column.

Science.gov (United States)

Narita, H; Takeda, Y; Takagaki, K; Nakamura, T; Harata, S; Endo, M

1995-11-20

Glycosaminoglycans (heparin, heparan sulfate, dermatan sulfate, chondroitin sulfate, and hyaluronic acid) were labeled with a fluorescent reagent, 2-aminopyridine. The fluoro-labeled glycosaminoglycans were subjected to high-performance liquid chromatography on a hydroxyapatite column. The binding property of each glycosaminoglycan to hydroxyapatite was different. The structural properties of glycosaminoglycans bound to hydroxyapatite were then investigated using chemical desulfated or enzymic depolymerized glycosaminoglycans. This revealed that the sulfate content and molecular weight of the glycosaminoglycans correlated with their binding properties to hydroxyapatite. Desulfated dermatan sulfate but not desulfated chondroitin 6-sulfate bound to the hydroxyapatite. These data indicate that iduronic acid residues of glycosaminoglycans are important for the binding property. The method described which uses hydroxyapatite columns facilitates rapid separation and microanalysis of the glycosaminoglycans, especially dermatan sulfate and chondroitin sulfate.

Mechanical, dielectric and surface analysis of hydroxyapatite doped anions for implantations

Science.gov (United States)

Helen, S.; Kumar, A. Ruban

2018-04-01

Calcium Phosphate has broad applications in field of medicine and in tissue engineering. In that hydroxyapatite is one of the calcium phosphate similar to bone and teeth mineral phase. The aim of this paper is to improve mechanical property of hydroxyapatite which has less mechanical strength by doping of ions. The ions increase its strength which can be used in various medical applications. Surface property of hydroxyapatite and electrical property of ion doped hydroxyapatite analyzed and shown that it can be used in implantations, coatings.

Highly transparent and conductive Al-doped ZnO nanoparticulate thin films using direct write processing

International Nuclear Information System (INIS)

Vunnam, S; Ankireddy, K; Kellar, J; Cross, W

2014-01-01

Solution processable Al-doped ZnO (AZO) thin films are attractive candidates for low cost transparent electrodes. We demonstrate here an optimized nanoparticulate ink for the fabrication of AZO thin films using scalable, low-cost direct write processing (ultrasonic spray deposition) in air at atmospheric pressure. The thin films were made via thermal processing of as-deposited films. AZO films deposited using the proposed nanoparticulate ink with further reducing in vacuum and rf plasma of forming gas exhibited optical transparency greater than 95% across the visible spectrum, and electrical resistivity of 0.5 Ω cm and it drops down to 7.0 × 10 −2 Ω cm after illuminating with UV light, which is comparable to commercially available tin doped indium oxide colloidal coatings. Various structural analyses were performed to investigate the influence of ink chemistry, deposition parameters, and annealing temperatures on the structural, optical, and electrical characteristics of the spray deposited AZO thin films. Optical micrographs confirmed the presence of surface defects and cracks using the AZO NPs ink without any additives. After adding N-(2-Aminoethyl)-3-aminopropylmethyldimethoxy silane to the ink, AZO films exhibited an optical transparency which was virtually identical to that of the plain glass substrate. (papers)

Electrophoretic deposition of zinc-substituted hydroxyapatite coatings.

Science.gov (United States)

Sun, Guangfei; Ma, Jun; Zhang, Shengmin

2014-06-01

Zinc-substituted hydroxyapatite nanoparticles synthesized by the co-precipitation method were used to coat stainless steel plates by electrophoretic deposition in n-butanol with triethanolamine as a dispersant. The effect of zinc concentration in the synthesis on the morphology and microstructure of coatings was investigated. It is found that the deposition current densities significantly increase with the increasing zinc concentration. The zinc-substituted hydroxyapatite coatings were analyzed by X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. It is inferred that hydroxyapatite and triethanolamine predominate in the chemical composition of coatings. With the increasing Zn/Ca ratios, the contents of triethanolamine decrease in the final products. The triethanolamine can be burnt out by heat treatment. The tests of adhesive strength have confirmed good adhesion between the coatings and substrates. The formation of new apatite layer on the coatings has been observed after 7days of immersion in a simulated body fluid. In summary, the results show that dense, uniform zinc-substituted hydroxyapatite coatings are obtained by electrophoretic deposition when the Zn/Ca ratio reaches 5%. Copyright © 2014 Elsevier B.V. All rights reserved.

Histologic analysis of a retrieved hydroxyapatite-coated femoral prosthesis

DEFF Research Database (Denmark)

Søballe, K; Gotfredsen, K; Brockstedt-Rasmussen, H

1991-01-01

A hydroxyapatite-coated hip hemi-prosthesis was retrieved from a 98-year-old osteoporotic woman 12 weeks after implantation. Histologic analysis revealed bone and fibrous tissue almost evenly distributed around the surface of the implant circumference. Quantitative histologic analysis showed...... that 48% of the hydroxyapatite surface was covered by bone. Fibrous tissue covered 30% of the prosthetic surface, and 20% of the surface had no tissue coverage. Scanning electron microscopy showed direct contact without any clear boundary between the newly formed bone and the hydroxyapatite ceramic....

Synthesis and release of trace elements from hollow and porous hydroxyapatite spheres

International Nuclear Information System (INIS)

Xia Wei; Grandfield, Kathryn; Schwenke, Almut; Engqvist, Haakan

2011-01-01

It is known that organic species regulate fabrication of hierarchical biological forms via solution methods. However, in this study, we observed that the presence of inorganic ions plays an important role in the formation and regulation of biological spherical hydroxyapatite formation. We present a mineralization method to prepare ion-doped hydroxyapatite spheres with a hierarchical structure that is free of organic surfactants and biological additives. Porous and hollow strontium-doped hydroxyapatite spheres were synthesized via controlling the concentration of strontium ions in a calcium and phosphate buffer solution. Similarly, fluoride and silicon-doped hydroxyapatite spheres were synthesized. While spherical particle formation was attainable at low and high temperature for Sr-doped hydroxyapatite, it was only possible at high temperature in the F/Si-doped system. The presence of inorganic ions not only plays an important role in the formation and regulation of biological spherical hydroxyapatite, but also could introduce pharmaceutical effects as a result of trace element release. Such ion release results showed a sustained release with pH responsive behavior, and significantly influenced the hydroxyapatite re-precipitation. These ion-doped hydroxyapatite spheres with hollow and porous structure could have promising applications as bone/tooth materials, drug delivery systems, and chromatography supports.

Surface fractal dimensions and textural properties of mesoporous alkaline-earth hydroxyapatites

International Nuclear Information System (INIS)

Vilchis-Granados, J.; Granados-Correa, F.; Barrera-Díaz, C.E.

2013-01-01

This work examines the surface fractal dimensions (D f ) and textural properties of three different alkaline-earth hydroxyapatites. Calcium, strontium and barium hydroxyapatite compounds were successfully synthesized via chemical precipitation method and characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectrometry, Fourier transform infrared spectroscopy, and N 2 -physisorption measurements. Surface fractal dimensions were determined using single N 2 -adsorption/desorption isotherms method to quantify the irregular surface of as-prepared compounds. The obtained materials were also characterized through their surface hydroxyl group content, determined by the mass titration method. It was found that the D f values for the three materials covered the range of 0.77 ± 0.04–2.33 ± 0.11; these results indicated that the materials tend to have smooth surfaces, except the irregular surface of barium hydroxyapatite. Moreover, regarding the synthesized calcium hydroxyapatite exhibited better textural properties compared with the synthesized strontium and barium hydroxyapatites for adsorbent purposes. However, barium hydroxyapatite shows irregular surface, indicating a high population of active sites across the surface, in comparison with the others studied hydroxyapatites. Finally, the results showed a linear correlation between the surface hydroxyl group content at the external surface of materials and their surface fractal dimensions.

Hydroxyapatite Reinforced Coatings with Incorporated Detonationally Generated Nanodiamonds

International Nuclear Information System (INIS)

Pramatarova, L.; Pecheva, E.; Hikov, T.; Fingarova, D.; Dimitrova, R.; Spassov, T.; Krasteva, N.; Mitev, D.

2010-01-01

We studied the effect of the substrate chemistry on the morphology of hydroxyapatite-detonational nanodiamond composite coatings grown by a biomimetic approach (immersion in a supersaturated simulated body fluid). When detonational nanodiamond particles were added to the solution, the morphology of the grown for 2 h composite particles was porous but more compact then that of pure hydroxyapatite particles. The nanodiamond particles stimulated the hydroxyapatite growth with different morphology on the various substrates (Ti, Ti alloys, glasses, Si, opal). Biocompatibility assay with MG63 osteoblast cells revealed that the detonational nanodiamond water suspension with low and average concentration of the detonational nanodiamond powder is not toxic to living cells.

Structural and dielectric properties of yttrium-substituted hydroxyapatites

Energy Technology Data Exchange (ETDEWEB)

Kaygili, Omer, E-mail: okaygili@firat.edu.tr [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey); Dorozhkin, Sergey V. [Kudrinskaja sq. 1-155, 123242 Moscow (Russian Federation); Ates, Tankut [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey); Canan Gursoy, N. [Department of Microbiology and Clinic Microbiology, Inonu University, 44280 Malatya (Turkey); Keser, Serhat [Department of Chemistry, Faculty of Science, Firat University, 23119 Elazig (Turkey); Yakuphanoglu, Fahrettin [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey); Birkan Selçuk, A. [Technology Department, Saraykoy Nuclear Research and Training Centre, 06983 Ankara (Turkey)

2015-02-01

Hydroxyapatite (HAp) samples doped with 0, 2 and 4 at.% of yttrium (Y) were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy attached with energy dispersive X-ray (EDX) spectroscopy, antimicrobial activity tests and dielectric studies. The hydroxyl groups observed in FTIR spectra confirmed the formation of HAp phase in the studied samples. The crystallite size, crystallinity degree and lattice parameters of the samples were changed with Y content. The volume of the unit cell was gradually decreased with the addition of Y. Undoped and Y-containing HAp samples were screened to determine their in vitro antimicrobial activities against the standard strains. It was found that no samples have any antimicrobial effect. The relative dielectric permittivity and dielectric loss are affected by Y content. While the alternating current conductivity increases with increasing frequency, it decreases with increasing Y content. - Highlights: • The lattice parameters and crystal size are affected by Y content. • The volume of the unit cell was gradually decreased with the addition of Y. • No samples have any antimicrobial effect. • The alternating current conductivity decreases with increasing Y content.

Structural and dielectric properties of yttrium-substituted hydroxyapatites

International Nuclear Information System (INIS)

Kaygili, Omer; Dorozhkin, Sergey V.; Ates, Tankut; Canan Gursoy, N.; Keser, Serhat; Yakuphanoglu, Fahrettin; Birkan Selçuk, A.

2015-01-01

Hydroxyapatite (HAp) samples doped with 0, 2 and 4 at.% of yttrium (Y) were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy attached with energy dispersive X-ray (EDX) spectroscopy, antimicrobial activity tests and dielectric studies. The hydroxyl groups observed in FTIR spectra confirmed the formation of HAp phase in the studied samples. The crystallite size, crystallinity degree and lattice parameters of the samples were changed with Y content. The volume of the unit cell was gradually decreased with the addition of Y. Undoped and Y-containing HAp samples were screened to determine their in vitro antimicrobial activities against the standard strains. It was found that no samples have any antimicrobial effect. The relative dielectric permittivity and dielectric loss are affected by Y content. While the alternating current conductivity increases with increasing frequency, it decreases with increasing Y content. - Highlights: • The lattice parameters and crystal size are affected by Y content. • The volume of the unit cell was gradually decreased with the addition of Y. • No samples have any antimicrobial effect. • The alternating current conductivity decreases with increasing Y content

The coprecipitation of strontium with hydroxyapatite

International Nuclear Information System (INIS)

Fujino, Osamu

1975-01-01

The distribution behavior of the strontium ion between hydroxyapatite and the parent solution was investigated. The hydroxyapatite was formed by the extremely slow addition of diammonium hydrogenphosphate to solutions of calcium and strontium nitrate buffered with ethylenediamine at 80 0 C. The precipitate yielded a typical X-ray diffraction pattern of hydroxyapatite and had a composition in which the Ca/P molar ratio was 1.67 at pH 6.80. The strontium ion was coprecipitated in the apatite, obeying the Doerner and Hoskins logarithnmic distribution law. The distribution coefficient was scarcely affected by the strontium concentration on the pH value in the parent solution, and had a value of 0.26+-0.02 at 80 0 C. On the other hand, the apparent distribution coefficient was a little affected by such organic anions as acetate, citrate, lactate, glycinate, and glutamate ions. The lattice constants of the precipitates prepared in the research were measured in order to confirm the formation of the solid solutions. (auth.)

Bio resorbability of the modified hydroxyapatite in Tris-HCL buffer

International Nuclear Information System (INIS)

Golovanova, O A; Izmailov, R R; Ghyngazov, S A

2016-01-01

The solubility of carbonated hydroxyapatite powders and granulated carbonated hydroxyapatite produced from the synovial biofluid model solution has been studied. The kinetic characteristics of dissolution were determined. It was found that the solubility of carbonated hydroxyapatite is higher as compared to that of hydroxyapatite. The impact of the organic matrix on the rate of sample dissolution was revealed. For HA-gelatin composites, as the gelatin concentration grows, the dissolution rate becomes greater, and a sample of 6.0 g / L concentration has higher resorbability. The results of the research can be used to study the kinetics of dissolution and the biocompatibility of ceramic materials for medicine, namely for reconstructive surgery, dentistry, and development of drug delivery systems. (paper)

Bacterial adhesion studies on titanium, titanium nitride and modified hydroxyapatite thin films

Energy Technology Data Exchange (ETDEWEB)

Jeyachandran, Y L [Department of Physics, Bharathiar University, Coimbatore 641 046, Tamil Nadu (India); Venkatachalam, S [Department of Physics, Bharathiar University, Coimbatore 641 046, Tamil Nadu (India); Karunagaran, B [Department of Physics, Bharathiar University, Coimbatore 641 046, Tamil Nadu (India); Narayandass, Sa K [Department of Physics, Bharathiar University, Coimbatore 641 046, Tamil Nadu (India); Mangalaraj, D [Department of Physics, Bharathiar University, Coimbatore 641 046, Tamil Nadu (India); Bao, C Y [West China College of Stomatology, Sichuan University, Chengdu 610041 (China); Zhang, C L [West China College of Stomatology, Sichuan University, Chengdu 610041 (China)

2007-01-15

A qualitative study on adhesion of the oral bacteria Porphyromonas gingivalis on titanium (Ti), titanium nitride (TiN), fluorine modified hydroxyapatite (FHA) and zinc modified FHA (Zn-FHA) thin films is investigated. Ti and TiN thin films were deposited by DC magnetron sputtering and hydroxyapatite-based films were prepared by solgel method. The crystalline structure, optical characteristics, chemical composition and surface topography of the films were studied by XRD, optical transmission, XPS, EDAX and AFM measurements. The predominant crystallite orientation in the Ti and TiN films was along (002) and (111) of hcp and cubic structures, respectively. The Ti : O : N composition ratio in the surface of the Ti and TiN films was found to be 7 : 21 : 1 and 3 : 8 : 2, respectively. The atomic concentration ratio (Zn + Ca) / P in Zn-FHA film was found to be 1.74 whereby the Zn replaced 3.2% of Ca. The rough surface feature in modified HA films was clearly observed in the SEM images and the surface roughness (rms) of Ti and TiN films was 2.49 and 3.5 nm, respectively, as observed using AFM. The film samples were sterilized, treated in the bacteria culture medium, processed and analyzed using SEM. Surface roughness of the films was found to have least influence on the bacterial adhesion. More bacteria were observed on the TiN film with oxide nitride surface layer and less number of adhered bacteria was noticed on the Ti film with native surface oxide layer and on Zn-FHA film.

Bacterial adhesion studies on titanium, titanium nitride and modified hydroxyapatite thin films

International Nuclear Information System (INIS)

Jeyachandran, Y.L.; Venkatachalam, S.; Karunagaran, B.; Narayandass, Sa.K.; Mangalaraj, D.; Bao, C.Y.; Zhang, C.L.

2007-01-01

A qualitative study on adhesion of the oral bacteria Porphyromonas gingivalis on titanium (Ti), titanium nitride (TiN), fluorine modified hydroxyapatite (FHA) and zinc modified FHA (Zn-FHA) thin films is investigated. Ti and TiN thin films were deposited by DC magnetron sputtering and hydroxyapatite-based films were prepared by solgel method. The crystalline structure, optical characteristics, chemical composition and surface topography of the films were studied by XRD, optical transmission, XPS, EDAX and AFM measurements. The predominant crystallite orientation in the Ti and TiN films was along (002) and (111) of hcp and cubic structures, respectively. The Ti : O : N composition ratio in the surface of the Ti and TiN films was found to be 7 : 21 : 1 and 3 : 8 : 2, respectively. The atomic concentration ratio (Zn + Ca) / P in Zn-FHA film was found to be 1.74 whereby the Zn replaced 3.2% of Ca. The rough surface feature in modified HA films was clearly observed in the SEM images and the surface roughness (rms) of Ti and TiN films was 2.49 and 3.5 nm, respectively, as observed using AFM. The film samples were sterilized, treated in the bacteria culture medium, processed and analyzed using SEM. Surface roughness of the films was found to have least influence on the bacterial adhesion. More bacteria were observed on the TiN film with oxide nitride surface layer and less number of adhered bacteria was noticed on the Ti film with native surface oxide layer and on Zn-FHA film

Biocompatibility of hydroxyapatite scaffolds processed by lithography-based additive manufacturing.

Science.gov (United States)

Tesavibul, Passakorn; Chantaweroad, Surapol; Laohaprapanon, Apinya; Channasanon, Somruethai; Uppanan, Paweena; Tanodekaew, Siriporn; Chalermkarnnon, Prasert; Sitthiseripratip, Kriskrai

2015-01-01

The fabrication of hydroxyapatite scaffolds for bone tissue engineering applications by using lithography-based additive manufacturing techniques has been introduced due to the abilities to control porous structures with suitable resolutions. In this research, the use of hydroxyapatite cellular structures, which are processed by lithography-based additive manufacturing machine, as a bone tissue engineering scaffold was investigated. The utilization of digital light processing system for additive manufacturing machine in laboratory scale was performed in order to fabricate the hydroxyapatite scaffold, of which biocompatibilities were eventually evaluated by direct contact and cell-culturing tests. In addition, the density and compressive strength of the scaffolds were also characterized. The results show that the hydroxyapatite scaffold at 77% of porosity with 91% of theoretical density and 0.36 MPa of the compressive strength are able to be processed. In comparison with a conventionally sintered hydroxyapatite, the scaffold did not present any cytotoxic signs while the viability of cells at 95.1% was reported. After 14 days of cell-culturing tests, the scaffold was able to be attached by pre-osteoblasts (MC3T3-E1) leading to cell proliferation and differentiation. The hydroxyapatite scaffold for bone tissue engineering was able to be processed by the lithography-based additive manufacturing machine while the biocompatibilities were also confirmed.

One-pot synthesis of a chitosan-based hydrogel as a potential device for magnetic biomaterial

International Nuclear Information System (INIS)

Paulino, Alexandre T.; Guilherme, Marcos R.; Almeida, Elisangela A.M.S. de; Pereira, Antonio G.B.; Muniz, Edvani C.; Tambourgi, Elias B.

2009-01-01

This describes the cross-linking/co-polymerization reaction of chitosan (CS), acrylic acid (AAc), and N, N'-methylenebisacrylamide (MBA) in the presence of citrate-covered-γ-Fe 2 O 3 nanoparticules. A gelling process was verified by means of spectroscopic methods; Fourier transform infrared (FT-IR) and solid-state 13 C-CP/MAS nuclear magnetic resonance (NMR). The corresponding signals of the gelling process, in the 13 C NMR spectra, for the magnetic hydrogel were shifted to lower values due to embedding of the citrate-covered-γ-Fe 2 O 3 nanoparticules. The X-ray diffraction (XRD) confirmed that the crystallinity of the magnetic hydrogel exhibited a different crystalline structure to that without magnetic properties. The Moessbauer and magnetization analysis revealed that the magnetic hydrogel displays a high lattice strain, due to bonded iron atom covalence and superparamagnetism. From scanning electronic microscope (SEM) micrographs, no separation phase coexists between the magnetic nanoparticules and cross-linked hydrogel, indicating an excellent dispersion throughout the hydrogel. The swelling rate was dependent on the cross-linking degree of the hydrogel and ionic strength of the aqueous solution.

Study of the fission products fixation in the hydroxyapatite mineral

International Nuclear Information System (INIS)

Soriano R, J. M.

2011-01-01

In this research work, sorption properties of hydroxyapatite in aqueous solutions were studied using Na + and K + ion behavior. In addition, the fission products 99 Tc and 107 Pd uptake was studied to determine their sorption mechanisms on hydroxyapatite. This research was conducted in two stages. The first stage aimed to identify surface reactive sites of hydroxyapatite surface. This surface study was performed by the radiotracer method using 24 Na and 42 K radionuclides and applying the ion-exchange theory. It provides evidence in terms of the saturation curves of individual behaviour of the Na + and K + cations. Hydroxyapatite reactive sites were identified and quantified from the results and application of the ion-exchange model: a mono-functional site of 0.28 mmol g -1 for the sodium hydroxylate form and a dipr otic site with two saturation curves of 0.14 mmol g -1 each, for the sodium phosphate form. In a second stage, the sorption of fission products, Tc and Pd, on hydroxyapatite was studied. This sorption was expressed in terms of distribution coefficients obtained with equivalent radiotracers: 99m Tc and 109 Pd. Tc presented a low sorption affinity on hydroxyapatite in aqueous medium 0.02 M NaH 2 PO 4 and the results also show that Tc is not sorbed from perchlorate medium (0.01 M Ca(ClO 4 ) 2 ). Sorption behaviour of Pd(II) on hydroxyapatite was studied for different experimental conditions, with parameter such as: ph, aqueous medium (0.01 M NaClO 4 , 0.01 M and 0.025 M Ca(ClO 4 ) 2 , and 0.02 M NaH 2 PO 4 ), the solid solution ratio (10, 4 and 0.020 g/L), and the palladium concentration were studied. Pd sorption was complete at solid-solution ratios 10 and 4 g/L. A strong sorption affinity of hydroxyapatite for palladium was obtained at solid-solution ratio 0.020 g/L. In the interpretation of the results it was considered the aqueous chemistry of palladium, solid dissolution, as well as the existence of reactive sites at the hydroxyapatite surface. The

Nanostructure of plasma-sprayed hydroxyapatite coating

International Nuclear Information System (INIS)

Suvorova, E.I.; Klechkovskaya, V.V.; Bobrovsky, V.V.; Khamchukov, Yu.D.; Klubovich, V.V.

2003-01-01

Calcium phosphate coatings were studied by high-resolution transmission microscopy, microdiffraction, and X-ray energy-dispersive spectroscopy. Coatings were prepared by spraying hydroxyapatite targets onto copper, nickel, and chromium substrates and onto NaCl and BaF 2 single crystals in an argon plasma at a gas pressure of ∼1 Pa; the sputter power was about 200 W; and the RF-generator frequency was 13.56 MHz. Under the conditions used, thin layers of nanocrystalline hydroxyapatite were formed regardless of the nature of the substrate

Antibacterial effects of silver-doped hydroxyapatite thin films sputter deposited on titanium

International Nuclear Information System (INIS)

Trujillo, Nathan A.; Oldinski, Rachael A.; Ma, Hongyan; Bryers, James D.; Williams, John D.; Popat, Ketul C.

2012-01-01

Since many orthopedic implants fail as a result of loosening, wear, and inflammation caused by repeated loading on the joints, coatings such as hydroxyapatite (HAp) on titanium with a unique topography have been shown to improve the interface between the implant and the natural tissue. Another serious problem with long-term or ideally permanent implants is infection. It is important to prevent initial bacterial colonization as existing colonies have the potential to become encased in an extracellular matrix polymer (biofilm) that is resistant to antibacterial agents. In this study, plasma-based ion implantation was used to examine the effects of pre-etching on plain titanium. Topographical changes to the titanium samples were examined and compared via scanning electron microscopy. Hydroxyapatite and silver-doped hydroxyapatite thin films were then sputter deposited on titanium substrates etched at − 700 eV. For silver-doped films, two concentrations of silver (∼ 0.5 wt.% and ∼ 1.5 wt.%) were used. Silver concentrations in the film were determined using energy dispersive X-ray spectroscopy. Hydroxyapatite film thicknesses were determined by measuring the surface profile using contact profilometry. Staphylococcus epidermidis and Pseudomonas aeruginosa adhesion studies were performed on plain titanium, titanium coated with hydroxyapatite, titanium coated with ∼ 0.5 wt.% silver-doped hydroxyapatite, and titanium coated with ∼ 1.5 wt.% silver-doped hydroxyapatite. Results indicate that less bacteria adhered to surfaces containing hydroxyapatite and silver; further, as the hydroxyapatite films delaminated, silver ions were released which killed bacteria in suspension. - Highlights: ► We have developed a combination of plasma-based ion implantation and ion beam sputter deposition technique. ► Silver-doped hydroxyapatite thin films on titanium were developed. ► The thin films showed the ability to control the concentration of silver that is doped within the

Speciation and Health Risks of Atmospheric Nanoparticulates

Science.gov (United States)

Nguyen, Kennedy

Exposure to air pollution causes several adverse health effects such as asthma, respiratory disease, cardiovascular disease, cancer, and premature death; and the San Joaquin Valley is one of the most heavily polluted regions in the US. The mountains that surround the valley allow air pollution, including particulate matter, to remain stagnant, prolonging the exposure of valley populations to it. The primary sources of particulate matter for this region are aluminosilicate dust from agricultural activities, and soot emissions from diesel trucks and vehicular traffic. A substantial fraction of emitted material is nanoparticulate matter (testing in cell culture studies, and correlation of particulate properties and sources with their negative health impacts. These results can help identify the sources of air pollution to prioritize for mitigation for the greatest health benefit. In addition, further chemical speciation can help monitor the results of such mitigation efforts. Here, natural particulate matter samples from Merced and Fresno, two cities in the San Joaquin Valley, were analyzed. Ultrafine particles present were 40 to 50 nm in diameter and mostly composed of aluminum, silicon, oxygen, and iron hydroxide. XAS data confirmed the presence of the aluminosilicate as smectite clay and the iron hydroxide as ferrihydrite. Furthermore, a chemical speciation study investigated industrial emissions of air particulate matter. Samples were analyzed using electron microscopy for elemental composition and size distribution, and found to contain fine metal particulates (lead and iron) that can lead to lung inflammation. From characterization data, in order to create a simplified proxy particle system for cell culture studies, amorphous silica particles were synthesized using a modified Stober Synthesis and coated with iron hydroxide. A range of iron hydroxide concentrations (0.06 to 1.63 mmol of iron per gram of silica) were used to test the effect of iron contamination on

Adsorption of citrate ions on hydroxyapatite synthesized by various methods

International Nuclear Information System (INIS)

Skwarek, E.; Janusz, W.; Sternik, D.

2014-01-01

The specific adsorption of citric acid ions at hydroxyapatite interface was investigated by the means of radioisotope method ( 14 C) as a function of citric acid ions concentration, NaCl concentration and pH. Application of the hydroxyapatite has become wide in the biomaterial field as the Ca 10 (OH) 2 (PO 4 ) 6 possess biocompatibility with human hard tissue. Hydroxyapatite was synthesized using three different methods. The physical properties of the resulting powder were characterized by DTA/TG, XRD, AFM and SEM microscopy. Physicochemical qualities characterizing the electrical double layer of the hydroxyapatite/NaCl solution interface were determined. The zeta potential and the adsorption of citric acid molecule were studied as a function of pH. The point of zero charge and the isoelectric point of samples were determined. Electrical double layer parameters of hydroxyapatite/NaCl interface are influenced by a synthesis method. The points pH pzc and pH IEP for sample 1 are pH pzc 7.5 and pH IEP 3; for sample 2 pH pzc 7.05 and pH IEP 3, for sample 3 pH pzc 6.7 and pH IEP 3. Temperature has weak influence both on pure substance and with citric acid adsorbed, as derivatographic analysis has shown, and characterization of hydroxyapatite structure may be carried out by this thermal analysis. Two phenomena are responsible for citric acid adsorption: phosphate group's replacement at hydroxyapatite surface by citric ions parallel to intraspherical complexes formation. (author)

Production and thermal stability of pure and Cr3+ -doped hydroxyapatite

International Nuclear Information System (INIS)

De Araujo, T S; De Souza, S O; De Sousa, E M B; Araujo, M S

2010-01-01

Hydroxyapatite (HAP) have been used as starting material for biomedical applications. The pure and Cr 3+ -doped hydroxyapatite were prepared by chemical precipitation reactions at 100, 500 e 800 0 C in order to investigate the thermal stability of these materials. The characterization of the thermal behavior of this phosphate, especially on the structural changes with heating, is very important for production of sunscreens The powders were characterized using chemical analysis: X-ray diffraction (XRD) and thermal analysis. The present study was successful in the preparation of pure hydroxyapatite and chromium substituted hydroxyapatites with good thermal stability and nanoparticles formation.

Peculiarities of hydroxyapatite/nanodiamond composites as novel implants

International Nuclear Information System (INIS)

Pramatarova, L; Dimitrova, R; Pecheva, E; Spassov, T; Dimitrova, M

2007-01-01

Hydroxyapatite/detonation nanodiamond composites are created on silica glass and cover glass by simple soaking process in an open deposition type set-up. The supersaturated solution (simulated body fluid, SBF) is prepared in a way to resemble the composition of human blood plasma. The composite growth is carried out through the addition of detonation nanodiamond particles to the SBF. Scanning electron microscopy, X-ray diffraction and FTIR spectroscopy are used to determine the surface morphology and the structure of the hydroxyapatite /detonation nanodiamond composite layers. The applied methods provide evidence that the nanodiamond surface functional groups interact strongly with the biological solution. The detonation nanodiamond surface is chemically multifunctional (surface OH, C-O-H, C = C, C-O-C and C = O groups exist), so that the hydroxyapatite is grown both by physical adsorption and chemical interaction. The OH - groups are regarded to play an important role in the hydroxyapatite growth on a diamond's surface from SBF, as they charge it negatively and attract Ca 2+ ions, which in turn attract PO 4 3- ions, thus forming apatite nuclei

In situ ring-opening polymerization of hydroxyapatite/poly (ethylene ...

Indian Academy of Sciences (India)

2016-08-26

Aug 26, 2016 ... Hydroxyapatite/poly(ethylene adipate)--poly(ethylene terephthalate) biomaterials (HAp/PEA--PET) have been prepared by ring opening polymerization (ROP) of cyclic oligo(ethylene adipate)--oligo(ethylene terephthalate) (C-OEA--C-OET) in the porous hydroxyapatite (HAp) scaffolds at 250 ...

Preparation and Characterization of Starch-g-PVA/Nano-hydroxyapatite Complex Hydrogel

Institute of Scientific and Technical Information of China (English)

无

2005-01-01

Starch-g-PVA/hydroxyapatite complex hydrogel was prepared with two-repeated freezing/ thawing circles. SEM observation results exhibits that hydroxyapatite is dispersed in starch-g-PVA in nanoscale. Thermogravimetric analysis curves show that the remained fraction keeps the same at the temperatures higher than 490℃ . It was found the dried starch-g- PVA/ hydroxyapatite films could reswell within 12 minutes.

The Effect of Zirconia in Hydroxyapatite on Staphylococcus epidermidis Growth

Directory of Open Access Journals (Sweden)

Widowati Siswomihardjo

2012-01-01

. Conclusion. The addition of zirconia into hydroxyapatite affected the growth of S. epidermidis. Hydroxyapatite with 20% zirconia proved to be an effective concentration to inhibit the growth of S. epidermidis colony.

Plasma Sprayed Hydroxyapatite Coatings: Influence of Spraying Power on Microstructure

International Nuclear Information System (INIS)

Mohd, S. M.; Abd, M. Z.; Abd, A. N.

2010-01-01

The plasma sprayed hydroxyapatite (HA) coatings are used on metallic implants to enhance the bonding between the implant and bone in human body. The coating process was implemented at different spraying power for each spraying condition. The coatings formed from a rapid solidification of molten and partly molten particles that impact on the surface of substrate at high velocity and high temperature. The study was concentrated on different spraying power that is between 23 to 31 kW. The effect of different power on the coatings microstructure was investigated using scanning electron microscope (SEM) and phase composition was evaluated using X-ray diffraction (XRD) analysis. The coatings surface morphology showed distribution of molten, partially melted particles and some micro-cracks. The produced coatings were found to be porous as observed from the cross-sectional morphology. The coatings XRD results indicated the presence of crystalline phase of HA and each of the patterns was similar to the initial powder. Regardless of different spraying power, all the coatings were having similar XRD patterns.

Chondroitin sulfate template-mediated biomimetic synthesis of nano-flake hydroxyapatite

Science.gov (United States)

He, Dan; Xiao, Xiufeng; Liu, Fang; Liu, Rongfang

2008-11-01

By Ca(NO 3) 2·4H 2O and (NH 4) 3PO 4·3H 2O as reagents and chondroitin sulfate (ChS) as a template, nano-flake hydroxyapatite (HA) is synthesized using a biomimetic method according to the biomineralization theory. HA crystals obtained are characterized in crystalline phase, microstructure, chemical composition and morphology by X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), transmission electron microscopy (TEM) and elemental analysis respectively. UV-vis spectrum is adopted to investigate interactions between functional groups ChS and HA. The results show that HA crystal nucleation and growth take place in chemical interactions between HA crystals and ChS as a template. And elemental analysis indicates that obtained HA contains a small amount of ChS. Furthermore, ChS concentration significantly affects the morphology of HA crystals. Staple-fiber-like HA crystals can be obtained at a low concentration in ChS, and flake-like HA crystals synthesized at a high concentration (≥0.5 wt.%) of ChS as a template.

Chondroitin sulfate template-mediated biomimetic synthesis of nano-flake hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

He Dan; Xiao Xiufeng; Liu Fang [College of Chemistry and Materials Science, Fujian Normal University, Fuzhou 350007 (China); Liu Rongfang [College of Chemistry and Materials Science, Fujian Normal University, Fuzhou 350007 (China)], E-mail: rfliu@vip.sina.com

2008-11-15

By Ca(NO{sub 3}){sub 2}.4H{sub 2}O and (NH{sub 4}){sub 3}PO{sub 4}.3H{sub 2}O as reagents and chondroitin sulfate (ChS) as a template, nano-flake hydroxyapatite (HA) is synthesized using a biomimetic method according to the biomineralization theory. HA crystals obtained are characterized in crystalline phase, microstructure, chemical composition and morphology by X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), transmission electron microscopy (TEM) and elemental analysis respectively. UV-vis spectrum is adopted to investigate interactions between functional groups ChS and HA. The results show that HA crystal nucleation and growth take place in chemical interactions between HA crystals and ChS as a template. And elemental analysis indicates that obtained HA contains a small amount of ChS. Furthermore, ChS concentration significantly affects the morphology of HA crystals. Staple-fiber-like HA crystals can be obtained at a low concentration in ChS, and flake-like HA crystals synthesized at a high concentration ({>=}0.5 wt.%) of ChS as a template.

Physico-chemical properties and solubility behaviour of multi-substituted hydroxyapatite powders containing silicon

International Nuclear Information System (INIS)

Sprio, S.; Tampieri, A.; Landi, E.; Sandri, M.; Martorana, S.; Celotti, G.; Logroscino, G.

2008-01-01

Hydroxyapatite powders characterized by ionic substitutions both in anionic and cationic sites were successfully prepared by synthesis in aqueous medium. The process parameters were set up to allow the simultaneous substitution of the foreign ions, namely carbonate, magnesium and silicon in the crystallographic site of calcium and phosphorus, keeping in count the competition which arises between atoms destined to occupy the same crystallographic site. The chemico-physical properties of the powders were investigated through several analytical techniques, i.e. X-ray diffraction, infrared spectroscopy, atomic emission spectroscopy and thermo-gravimetric analysis. The results show that the utilization of sodium hydrogen-carbonate as a reactant allows the entering of carbonate into the HA structure, mainly in phosphate position, while sodium is eliminated during the process of the powder washing. The entering of silicon in the HA structure progressively reduces its crystallinity, as also carbonate ions do. Silicate and carbonate ions can enter simultaneously into the HA structure, in biological-like amounts, although they compete for the occupation of the phosphate site; the powder crystallinity is strongly reduced as the content of the two substituting ions increases, so that a limit molar concentration exists where the apatite structure collapses and an amorphous phase forms with the simultaneous formation of crystalline calcium carbonate. Solubility tests, carried out at physiological conditions, reveal an increased calcium release in the HA powders containing silicon compared to the silicon-free HA; the solubility behaviour of the multi-substituted HA powders at physiological conditions makes these materials promising as bioactive bone scaffold, as they are able to continuously supply ions which are essential for the process of bone reconstruction

Cytotoxicity of nano-hydroxyapatite on human-derived oral epithelium cell line: an in vitro study

OpenAIRE

Farid Abassi; Mandana Sattari; Noushin Jalayer Naderi; Marzie Sorooshzadeh

2016-01-01

Background: Hydroxyapatite nanoparticles have a more surface contact and solubility than conventional hydroxyapatite. Hydroxynanoparticles enhances the biological and mechanical properties of new regenerated tissues. The hydroxyapatite nanoparticles have received attention as a new and effective osseous graft for using as scaffolds in bone regeneration. The reports on hydroxyapatite nanoparticles biocompatibility are controversial. It has been shown that hydroxyapatite nanoparticles induces i...

High quality aluminium doped zinc oxide target synthesis from nanoparticulate powder and characterisation of sputtered thin films

Energy Technology Data Exchange (ETDEWEB)

Isherwood, P.J.M., E-mail: P.J.M.Isherwood@lboro.ac.uk [Centre for Renewable Energy Systems Technology, Loughborough University, Loughborough, Leicestershire LE11 3TU (United Kingdom); Neves, N. [Innovnano, S. A., Rua Coimbra Inovação Parque, IParque Lote 13, 3040-570 Antanhol, Coimbra (Portugal); Bowers, J.W. [Centre for Renewable Energy Systems Technology, Loughborough University, Loughborough, Leicestershire LE11 3TU (United Kingdom); Newbatt, P. [Innovnano, S. A., Rua Coimbra Inovação Parque, IParque Lote 13, 3040-570 Antanhol, Coimbra (Portugal); Walls, J.M. [Centre for Renewable Energy Systems Technology, Loughborough University, Loughborough, Leicestershire LE11 3TU (United Kingdom)

2014-09-01

Nanoparticulate aluminium-doped zinc oxide powder was synthesised through detonation and subsequent rapid quenching of metallic precursors. This technique allows for precise compositional control and rapid nanoparticle production. The resulting powder was used to form sputter targets, which were used to deposit thin films by radio frequency sputtering. These films show excellent sheet resistance and transmission values for a wide range of deposition temperatures. Crystal structure analysis shows that crystals in the target have a random orientation, whereas the crystals in the films grow perpendicular to the substrate surface and propagate preferentially along the (002) axis. Higher temperature deposition reduces crystal quality with a corresponding decrease in refractive index and an increase in sheet resistance. Films deposited between room temperature and 300 °C were found to have sheet resistances equivalent to or better than indium tin oxide films for a given average transmission value. - Highlights: • Nanoparticulate AZO powder was used to produce sputter targets. • The powder synthesis technique allows for precise compositional control. • Sputtered films show excellent optical, electronic and structural properties. • High temperature films show reduced electrical and structural quality. • For a given transmission, films show equivalent sheet resistances to ITO.

Carbon foam/hydroxyapatite coating for carbon/carbon composites: Microstructure and biocompatibility

Energy Technology Data Exchange (ETDEWEB)

Zhang, Leilei, E-mail: zhangleilei1121@aliyun.com; Li, Hejun; Li, Kezhi; Zhang, Shouyang; Lu, Jinhua; Li, Wei; Cao, Sheng; Wang, Bin

2013-12-01

To improve the surface biocompatibility of carbon/carbon composites, a carbon foam/hydroxyapatite coating was applied using a combination method of slurry procedure and ultrasound-assisted electrochemical deposition procedure. The morphology, microstructure and chemical composition of the coating were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and X-ray diffraction. The biocompatibility of the carbon foam/hydroxyapatite coating was investigated by osteoblast-like MG63 cell culture tests. The results showed that the carbon foam could provide a large number of pores on the surface of carbon/carbon composites. The hydroxyapatite crystals could infiltrate into the pores and form the carbon foam/hydroxyapatite coating. The coating covered the carbon/carbon composites fully and uniformly with slice morphology. The cell response tests showed that the MG63 cells on carbon foam/hydroxyapatite coating had a better cell adhesion and cell proliferation than those on uncoated carbon/carbon composites. The carbon foam/hydroxyapatite coatings were cytocompatible and were beneficial to improve the biocompatibility. The approach presented here may be exploited for fabrication of carbon/carbon composite implant surfaces.

Carbon foam/hydroxyapatite coating for carbon/carbon composites: Microstructure and biocompatibility

International Nuclear Information System (INIS)

Zhang, Leilei; Li, Hejun; Li, Kezhi; Zhang, Shouyang; Lu, Jinhua; Li, Wei; Cao, Sheng; Wang, Bin

2013-01-01

To improve the surface biocompatibility of carbon/carbon composites, a carbon foam/hydroxyapatite coating was applied using a combination method of slurry procedure and ultrasound-assisted electrochemical deposition procedure. The morphology, microstructure and chemical composition of the coating were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and X-ray diffraction. The biocompatibility of the carbon foam/hydroxyapatite coating was investigated by osteoblast-like MG63 cell culture tests. The results showed that the carbon foam could provide a large number of pores on the surface of carbon/carbon composites. The hydroxyapatite crystals could infiltrate into the pores and form the carbon foam/hydroxyapatite coating. The coating covered the carbon/carbon composites fully and uniformly with slice morphology. The cell response tests showed that the MG63 cells on carbon foam/hydroxyapatite coating had a better cell adhesion and cell proliferation than those on uncoated carbon/carbon composites. The carbon foam/hydroxyapatite coatings were cytocompatible and were beneficial to improve the biocompatibility. The approach presented here may be exploited for fabrication of carbon/carbon composite implant surfaces.

Recycled hydroxyapatite coatings on 316L stainless steel substrates

International Nuclear Information System (INIS)

Mendes Filho, Antonio Alves; Pereira, Renato Alves; Araujo, Fernando Gabriel da Silva; Sousa, Camila Mateus de

2010-01-01

In this work were evaluated recycled hydroxyapatite coatings on 316L stainless steel substrates by plasma thermal aspersion. The hydroxyapatite used was obtained from bovine bone by the hydrothermal method. The samples of hydroxyapatite powders were divided according to their particle size distribution. The adhesion of the powders coating to the substrate was evaluated by assay scratch. The X-ray diffraction techniques and scanning electron microscopy were also used. The results of scratch resistance were between 46N and 63N. Analysis by scanning electron microscopy and x-ray diffraction showed no cracks coatings, single-phase and with few fused particles. (author)

Functionalization of the hydroxyapatite nanoparticles surface: source of new applications

International Nuclear Information System (INIS)

Rojas Sanchez, Leonardo

2012-01-01

The surface of the nano-calcium hydroxyapatite, Ca 10 (PO 4 ) 6 (OH) 2 is reacted with stearic acid, succinic anhydride, succinimide and 2 a minoetil dihydrogenphosphate. Introduction of different functional groups is given onto the surface. An ionic interaction is identified by infrared spectroscopy and Raman between the carboxylate groups of the resulting organic molecules and calcium of the hydroxyapatite. The formation of a P-O-P pyrophosphate type bond has been for 2-aminoethyl dihydrogen phosphate with hydroxyapatite groups. Hydroxyapatite phase was remained in all cases after the reaction as demonstrated by diffraction of x-ray in powder. The amount of spiked molecules is quantified by analysis of thermal degradation which together with the determination of the surface area by BET isotherms of nitrogen adsorption. A degree of surface coverage is estimated by the organic molecules. A maximum percentage of 71% is obtained for the functionalization with succinic anhydride, followed by 57% for the reaction with stearic acid. Dilute suspensions of different materials were prepared for which in phosphate buffer solution have presented two populations around 2 and 5 μm in diameter for the modified particles. The ζ-Potential of various materials was determined occurring a variation in the potential of the unmodified hydroxyapatite. The particles with physicochemical properties different of the starting hydroxyapatite were obtained, this has expanded the range of application of the material. (author) [es

On the assessment of hydroxyapatite fluoridation by means of Raman scattering

International Nuclear Information System (INIS)

Campillo, M.; Valiente, M.; Lacharmoise, P. D.; Reparaz, J. S.; Goni, A. R.

2010-01-01

Hydroxyapatite is the main mineral component of bones and teeth. Fluorapatite, a bioceramic that can be obtained from hydroxyapatite by chemical substitution of the hydroxide ions with fluoride, exhibits lower mineral solubility and larger mechanical strength. Despite the widespread use of fluoride against caries, a reliable technique for unambiguous assessment of fluoridation in in vitro tests is still lacking. Here we present a method to probe fluorapatite formation in fluoridated hydroxyapatite by combining Raman scattering with thermal annealing. In synthetic minerals, we found that effectively fluoride substituted hydroxyapatite transforms into fluorapatite only after heat treatment, due to the high activation energy for this first order phase transition.

On the assessment of hydroxyapatite fluoridation by means of Raman scattering

Science.gov (United States)

Campillo, M.; Lacharmoise, P. D.; Reparaz, J. S.; Goñi, A. R.; Valiente, M.

2010-06-01

Hydroxyapatite is the main mineral component of bones and teeth. Fluorapatite, a bioceramic that can be obtained from hydroxyapatite by chemical substitution of the hydroxide ions with fluoride, exhibits lower mineral solubility and larger mechanical strength. Despite the widespread use of fluoride against caries, a reliable technique for unambiguous assessment of fluoridation in in vitro tests is still lacking. Here we present a method to probe fluorapatite formation in fluoridated hydroxyapatite by combining Raman scattering with thermal annealing. In synthetic minerals, we found that effectively fluoride substituted hydroxyapatite transforms into fluorapatite only after heat treatment, due to the high activation energy for this first order phase transition.

Biomineralizing synthesis of mesoporous hydroxyapatite-calcium pyrophosphate polycrystal using ovalbumin as biosurfactant

International Nuclear Information System (INIS)

Zhao Hongshi; He Wen; Wang Yingjun; Yue Yuanzheng; Gao Xingguo; Li Zhengmao; Yan Shunpu; Zhou Weijia; Zhang Xudong

2008-01-01

Mesoporous polycrystals of hydroxyapatite-calcium pyrophosphate (HA-CPP) are synthesized via a biomineralizing route using ovalbumin as natural biosurfactant. The mesoporous structure of HA-CPP is characterized by means of X-ray diffraction (XRD), N 2 adsorption-desorption isotherms (NADI), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), atom force microscopy (AFM), polarization microscopy (PLM) and stereomicroscopy. The results show that the crystalline grains with an average diameter of 13.2 nm are uniformly distributed along the protein molecule chains, and this results in microsphere-like particles with diameters of 200-300 nm. The highly ordered pores involved in microspheres are found to be approximately 6.6 nm by small-angle XRD. The formation of lyotropic calcium liquid crystal (CLC) plays a key role in the formation and stabilization of the mesoporous structure. A schematic illustration is used to reveal the mechanism of protein-medicated HA-CPP biomineralization, which employs the protein tertiary structure to explain the formation of the porous particles

[Synthesis and characterization of CO-3(2-) doping nano-hydroxyapatite].

Science.gov (United States)

Liao, Jian-Guo; Li, Yan-Qun; Duan, Xing-Ze; Liu, Qiong

2014-11-01

CO3(2-) doping is an effective method to increase the biological activity of nano-hydroxyapatite (n-HA). In the present study, calcium nitrate and trisodium phosphate were chosen as raw materials, with a certain amount of Na2CO3 as a source of CO-3(2-) ions, to synthesize nano-carbonate hydroxyapatite (n-CHA) slurry by solution precipitation method. The structure and micro-morphology of n-CHA were characterized by transmission electron microscope (TEM), X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FTIR) and Raman spectroscopy (RS). The results revealed that the synthetic n-HA crystals are acicular in nanometer scale and have a crystal size of 20-30 nm in diameter and 60-80 nm in length, which are similar to natural bone apatite. And the crystallinity of n-CHA crystals decreases to the increment of CO3(2-). Samples with more CO3(2) have composition and structure more similar to the bone apatite. The value of lattice parameters a decreases, value of c increases, and c/a value increases with the increase in the amount of CO3(2-), in accordance with crystal cell parameters change rule of type B replacement. In the AB mixed type (substitution OH- and PO4(3-)) CHA, IR characteristic peak of CO3(2-) out-of-plane bending vibration appears at 872 cm(-1), meanwhile, the asymmetry flexible vibration band is split into band at 1 454 cm(-1) and band at 1 420 cm(-1), while weak CO3(2)-peak appears at 1 540 cm(-1). CO3(2-) Raman peak of symmetric stretching vibration appears at 1 122 cm(-1). CO3(2-) B-type (substitution PO4(3-)) peak appeared at 1 071 cm(-1). Through the calculation of integral area ratio of PO4(3-)/ CO3(2-), OH-/CO3(2-), and PO4(3-)/OH-, low quantity CO3(2-) is B-type and high quantity CO3(2-) is A-type (substitution OH-). The results show that the synthesized apatite crystals are AB hybrid substitued nano-carbonate hydroxyapatite, however B-type replacement is the main substitute mode. Due to similarity inthe shape, size, crystal structure

Optimization of nanoparticulate indium tin oxide slurries for the manufacture of ultra-thin indium tin oxide coatings with the slot-die coating process

International Nuclear Information System (INIS)

Wegener, M.; Riess, K.; Roosen, A.

2016-01-01

This paper deals with the optimization of colloidal processing to achieve suitable nanoparticulate indium tin oxide (ITO) slurries for the production of sub-μm-thin ITO coatings with the slot die coating process. For application in printed electronics these ITO coatings, which are composite films consisting of nanoparticulate ITO and a polymeric binder, should offer high flexibility, transparency and electrical conductivity. To preserve their flexibility, the composite films are not subject to any heat treatment, instead they are used as deposited and dried. To achieve very good transparency and electrical conductivity at the same time, the slurries must exhibit excellent dispersivity to result in a dense particle packing during film formation and drying. To reduce materials costs, films with thicknesses of several 100 nm are of interest. Therefore, the slot-die technique was applied as a fast, pre-dosing technique to produce sub-μm-thin ITO/binder composite films. The resulting ITO/binder films were characterized with regard to their key properties such as total transmission and specific electrical resistance. With the colloidal optimization of ethanol- and water-based nanoparticulate ITO slurries using PVP and PVB as binders, it was possible to achieve films of 250 nm in thickness exhibiting high total transmission of ∝ 93 % and a low specific electrical resistance of ∝ 10 Ω.cm.

Optimization of nanoparticulate indium tin oxide slurries for the manufacture of ultra-thin indium tin oxide coatings with the slot-die coating process

Energy Technology Data Exchange (ETDEWEB)

Wegener, M.; Riess, K.; Roosen, A. [Erlangen-Nuremberg Univ., Erlangen (Germany). Dept. of Materials Science, Glass and Ceramics

2016-07-01

This paper deals with the optimization of colloidal processing to achieve suitable nanoparticulate indium tin oxide (ITO) slurries for the production of sub-μm-thin ITO coatings with the slot die coating process. For application in printed electronics these ITO coatings, which are composite films consisting of nanoparticulate ITO and a polymeric binder, should offer high flexibility, transparency and electrical conductivity. To preserve their flexibility, the composite films are not subject to any heat treatment, instead they are used as deposited and dried. To achieve very good transparency and electrical conductivity at the same time, the slurries must exhibit excellent dispersivity to result in a dense particle packing during film formation and drying. To reduce materials costs, films with thicknesses of several 100 nm are of interest. Therefore, the slot-die technique was applied as a fast, pre-dosing technique to produce sub-μm-thin ITO/binder composite films. The resulting ITO/binder films were characterized with regard to their key properties such as total transmission and specific electrical resistance. With the colloidal optimization of ethanol- and water-based nanoparticulate ITO slurries using PVP and PVB as binders, it was possible to achieve films of 250 nm in thickness exhibiting high total transmission of ∝ 93 % and a low specific electrical resistance of ∝ 10 Ω.cm.

In situ ring-opening polymerization of hydroxyapatite/poly (ethylene ...

Indian Academy of Sciences (India)

Hydroxyapatite/poly(ethylene adipate)--poly(ethylene terephthalate) biomaterials (HAp/PEA--PET) have been prepared by ring opening polymerization (ROP) of cyclic oligo(ethylene adipate)--oligo(ethylene terephthalate) (C-OEA--C-OET) in the porous hydroxyapatite (HAp) scaffolds at 250 °C for 24 h under ...

Structure-property relationships of iron-hydroxyapatite ceramic matrix nanocomposite fabricated using mechanosynthesis method.

Science.gov (United States)

Nordin, Jamillah Amer; Prajitno, Djoko Hadi; Saidin, Syafiqah; Nur, Hadi; Hermawan, Hendra

2015-06-01

Hydroxyapatite (HAp) is an attractive bioceramics due to its similar composition to bone mineral and its ability to promote bone-implant interaction. However, its low strength has limited its application as load bearing implants. This paper presented a work focusing on the improvement of HAp mechanical property by synthesizing iron (Fe)-reinforced bovine HAp nanocomposite powders via mechanosynthesis method. The synthesis process was performed using high energy milling at varied milling time (3, 6, 9, and 12h). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM). Its mechanical properties were investigated by micro-Vicker's hardness and compression tests. Results showed that milling time directly influenced the characteristics of the nanocomposite powders. Amorphous BHAp was formed after 9 and 12h milling in the presence of HPO4(2-) ions. Continuous milling has improved the crystallinity of Fe without changing the HAp lattice structure. The nanocomposite powders were found in spherical shape, agglomerated and dense after longer milling time. The hardness and Young's modulus of the nanocomposites were also increased at 69% and 66%, respectively, as the milling time was prolonged from 3 to 12h. Therefore, the improvement of the mechanical properties of nanocomposite was attributed to high Fe crystallinity and homogenous, dense structure produced by mechanosynthesis. Copyright © 2015 Elsevier B.V. All rights reserved.

Toxoplasmose : une nouvelle approche vaccinale à base de nanoparticules d’amidon donne des résultats prometteurs

OpenAIRE

Le Rouzic, Jacques

2015-01-01

Pour lutter contre la toxoplasmose chez les ovins, des chercheurs de l’INRA, de l’Université de Tours et de la Faculté de Médecine de Lille ont développé une nouvelle approche vaccinale, utilisant des nanoparticules d’amidon et une administration par voie muqueuse. Cette approche ouvre de nouvelles perspectives vers des vaccins plus sûrs et plus efficaces.

The effect of carbonate on neptunium sorption by hydroxyapatite

International Nuclear Information System (INIS)

Moore, R.C.; Holt, K.

2005-01-01

Full text of publication follows: Hydroxyapatite, Ca 10 (PO 4 ) 6 (OH) 2 , is a common mineral, the main inorganic compound in bone and exhibits strong sorptive properties for many radionuclides. It has been widely studied and proposed as a backfill material for nuclear waste repositories. Neptunium is one the radionuclides sorbed by hydroxyapatite. Neptunium is of particular importance to nuclear waste repository performance because of its relatively high aqueous solubility, high mobility in the environment and long half-life. In this work, we report on the effects of carbonate on sorption of neptunium by hydroxyapatite. Batch sorption and desorption studies for neptunium were performed as a function of carbonate concentration in water using a synthetic hydroxyapatite. The results indicate even low concentrations of carbonate significantly reduce neptunium sorption and enhance desorption. The data were fit to several simple isotherm equations with the Langmuir equation giving the best results. The results of the work are discussed with respect to nuclear waste repository performance. (authors)

In-situ deposition of hydroxyapatite on graphene nanosheets

OpenAIRE

Neelgund, Gururaj M.; Oki, Aderemi; Luo, Zhiping

2013-01-01

Graphene nanosheets were effectively functionalized by in-situ deposition of hydroxyaptite through a facile chemical precipitation method. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. The resulting hydroxyapatite functionalized graphene nanosheets were characterized by attenuated total reflection IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, trans...

Nanoparticulation improves bioavailability of Erlotinib.

Science.gov (United States)

Yang, Kyung Mi; Shin, In Chul; Park, Joo Won; Kim, Kab-Sig; Kim, Dae Kyong; Park, Kyungmoon; Kim, Kunhong

2017-09-01

Nanoparticulation using fat and supercritical fluid (NUFS TM ) is a drug delivery platform technology enabling efficient and effective formulation of poorly soluble drugs. We performed experiments to examine whether NUFS™ could improve poor bioavailability and reduce fed-fasted bioavailability variances of erlotinib (Ert). NUFS-Ert was prepared using NUFS™ technology; its physical properties were characterized, and drug release was measured. Furthermore, in vitro and in vivo efficacy tests and pharmacokinetic analysis were performed. NUFS-Ert nanoparticles had an average size of 250 nm and were stable for 2 months at 40 °C, 4 °C, and room temperature. The dissolution rate of NUFS-Ert increased in bio-relevant dissolution media. NUFS-Ert was more potent in inhibiting EGF signaling and in suppressing the proliferation of A549, a human non-small cell lung cancer cell line. Furthermore, A549 xenografts in BALB/c nude mice treated with NUFS-Ert regressed more efficiently than those in the mice treated with vehicle or Tarceva ® . In addition, experimental lung metastasis was more efficiently inhibited by NUFS-Ert than by Tarceva ® . The relative bioavailability of NUFS-Ert compared with that of Tarceva ® was 550% and the ratio of the area under the concentration-time curve (AUC) of fed state to the AUC of fasted state was 1.8 for NUFS-Ert and 5.8 for Tarceva ® . NUFS-Ert could improve poor bioavailability and reduce fed-fasted bioavailability variances of Ert. NUFS-Ert was more efficacious than Tarceva ® .

Surface free energy predominates in cell adhesion to hydroxyapatite through wettability.

Science.gov (United States)

Nakamura, Miho; Hori, Naoko; Ando, Hiroshi; Namba, Saki; Toyama, Takeshi; Nishimiya, Nobuyuki; Yamashita, Kimihiro

2016-05-01

The initial adhesion of cells to biomaterials is critical in the regulation of subsequent cell behaviors. The purpose of this study was to investigate a mechanism through which the surface wettability of biomaterials can be improved and determine the effects of biomaterial surface characteristics on cellular behaviors. We investigated the surface characteristics of various types of hydroxyapatite after sintering in different atmospheres and examined the effects of various surface characteristics on cell adhesion to study cell-biomaterial interactions. Sintering atmosphere affects the polarization capacity of hydroxyapatite by changing hydroxide ion content and grain size. Compared with hydroxyapatite sintered in air, hydroxyapatite sintered in saturated water vapor had a higher polarization capacity that increased surface free energy and improved wettability, which in turn accelerated cell adhesion. We determined the optimal conditions of hydroxyapatite polarization for the improvement of surface wettability and acceleration of cell adhesion. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and characterization of a nanostructured matrix hydroxyapatite ceramic bone reconstruction

International Nuclear Information System (INIS)

Correa, P.; Camargo, N.H.A.; Silva, D.F.

2012-01-01

The nanostructured ceramics have been shown promise as biomaterials for bone reconstruction. Among calcium phosphates, hydroxyapatite Ca/P ratio = 1.67 mol stands out because of its crystallographic similarity with the mineral bone phase and biocompatibility. This work was based on synthesis and characterization of a nanostructured hydroxyapatite for use in reconstituting bone tissue. The synthesis method for obtaining the bioceramic powder occurred at process of dissolution/precipitation, involving CaO solid/liquid and phosphoric acid required for forming the composition of Ca/P = 1.67 mole. The material recovered from the synthesis was calcined at 900 ° C/2h, providing the hydroxyapatite powder nanometer. This was subjected to mechanical fragmentation process in mill attritor, providing a hydroxyapatite with modified surface morphology. The results presented relate to morphological characterization studies (SEM), mineralogical (XRD), chemical (FTIR) and particle size distribution, using the laser particle size analysis method. Such results showed the formation of hydroxyapatite phase and morphology satisfactory for use in reconstituting bone tissue

Analysis of the structure, particle morphology and photoluminescent properties of ZnS:Mn2+ nanoparticulate phosphors

CSIR Research Space (South Africa)

Raleaooa, PV

2018-01-01

Full Text Available stream_source_info Raleaooa_20160_2018.pdf.txt stream_content_type text/plain stream_size 1286 Content-Encoding UTF-8 stream_name Raleaooa_20160_2018.pdf.txt Content-Type text/plain; charset=UTF-8 Optik - International... journal for Light and Electron Optics Analysis of the structure, particle morphology and photoluminescent properties of ZnS:Mn2+ nanoparticulate phosphors Raleaooa PV Roodt A Mhlongo GH Motaung DE Ntwaeaborwa OM ABSTRACT: The structure...

Comparison of hydroxyapatite and dental enamel for testing shear bond strengths.

Science.gov (United States)

Imthiaz, Nishat; Georgiou, George; Moles, David R; Jones, Steven P

2008-05-01

To investigate the feasibility of using artificial hydroxyapatite as a future biomimetic laboratory substitute for human enamel in orthodontic bond strength testing by comparing the shear bond strengths and nature of failure of brackets bonded to samples of hydroxyapatite and enamel. One hundred and fifty hydroxyapatite discs were prepared by compression at 20 tons and fired in a furnace at 1300 degrees C. One hundred and five enamel samples were prepared from the buccal and palatal/lingual surfaces of healthy premolars extracted for orthodontic purposes. Orthodontic brackets were bonded to each sample and these were subjected to shear bond strength testing using a custom-made jig mounted in an Instron Universal Testing Machine. The force value at bond failure was obtained, together with the nature of failure which was assessed using the Adhesive Remnant Index. The mean shear bond strength for the enamel samples was 16.62 MPa (95 per cent CI: 15.26, 17.98) and for the hydroxyapatite samples 20.83 MPa (95 per cent CI: 19.68, 21.98). The difference between the two samples was statistically significant (p enamel samples scored 2 or 3, while 49 per cent of the hydroxyapatite samples scored 0 or 1. Hydroxyapatite was an effective biomimetic substrate for bond strength testing with a mean shear bond strength value (20.83 MPa) at the upper end of the normal range attributed to enamel (15-20 MPa). Although the difference between the shear bond strengths for hydroxyapatite and enamel was statistically significant, hydroxyapatite could be used as an alternative to enamel for comparative laboratory studies until a closer alternative is found. This would eliminate the need for extracted teeth to be collected. However, it should be used with caution for quantitative studies where true bond strengths are to be investigated.

Peculiarities of hydroxyapatite/nanodiamond composites as novel implants

Energy Technology Data Exchange (ETDEWEB)

Pramatarova, L [Georgi Nadjakov Institute of Solid State Physics, Bulgarian Academy of Sciences (Bulgaria); Dimitrova, R [Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences (Bulgaria); Pecheva, E [Georgi Nadjakov Institute of Solid State Physics, Bulgarian Academy of Sciences (Bulgaria); Spassov, T [Sofia University, Faculty of Chemistry (Bulgaria); Dimitrova, M [Georgi Nadjakov Institute of Solid State Physics, Bulgarian Academy of Sciences (Bulgaria)

2007-12-15

Hydroxyapatite/detonation nanodiamond composites are created on silica glass and cover glass by simple soaking process in an open deposition type set-up. The supersaturated solution (simulated body fluid, SBF) is prepared in a way to resemble the composition of human blood plasma. The composite growth is carried out through the addition of detonation nanodiamond particles to the SBF. Scanning electron microscopy, X-ray diffraction and FTIR spectroscopy are used to determine the surface morphology and the structure of the hydroxyapatite /detonation nanodiamond composite layers. The applied methods provide evidence that the nanodiamond surface functional groups interact strongly with the biological solution. The detonation nanodiamond surface is chemically multifunctional (surface OH, C-O-H, C = C, C-O-C and C = O groups exist), so that the hydroxyapatite is grown both by physical adsorption and chemical interaction. The OH{sup -} groups are regarded to play an important role in the hydroxyapatite growth on a diamond's surface from SBF, as they charge it negatively and attract Ca{sup 2+} ions, which in turn attract PO{sub 4}{sup 3-} ions, thus forming apatite nuclei.

Scaffolds of polycaprolactone with hydroxyapatite fibers

International Nuclear Information System (INIS)

Cardoso, Guinea B.C.; Zavaglia, Cecilia A.C.; Arruda, Antonio Celso F.

2009-01-01

Scaffolds of poly (ε-caprolactone) has been studied in many researches in tissue engineering. The used of hydroxyapatite fibers, allowed increase its resistance mechanical, beside the character bioactive and osteoconductive. Improving, its role in tissue engineering. The aim in this study was developed polycaprolactone matrix with dispersed hydroxyapatite fibers. The characterizations were by scanning electron microscopy (SEM), X- Ray Diffractometer (XRD), X-Ray Fluorescence (XRF) and Energy dispersive X-Ray Detector (EDX). Was able reviewed its composition, morphology and possible contaminations. The results were scaffolds with porosity and distribution of the fibers in all its area. (author)

Water-based sol-gel synthesis of hydroxyapatite: process development.

Science.gov (United States)

Liu, D M; Troczynski, T; Tseng, W J

2001-07-01

Hydroxyapatite (HA) ceramics were synthesized using a sol-gel route with triethyl phosphite and calcium nitrate as phosphorus and calcium precursors, respectively. Two solvents, water and anhydrous ethanol, were used as diluting media for HA sol preparation. The sols were stable and no gelling occurred in ambient environment for over 5 days. The sols became a white gel only after removal of the solvents at 60 degrees C. X-ray diffraction showed that apatitic structure first appeared at a temperature as low as 350 degrees C. The crystal size and the HA content in both gels increase with increasing calcination temperature. The type of initial diluting media (i.e., water vs. anhydrous ethanol) did not affect the microstructural evolution and crystallinity of the resulting HA ceramic. The ethanol-based sol dip-coated onto a Ti substrate, followed by calcination at 450 degrees C, was found to be porous with pore size ranging from 0.3 to 1 microm. This morphology is beneficial to the circulation of physiological fluid when the coating is used for biomedical applications. The satisfactory adhesion between the coating and substrate suggests its suitability for load-bearing uses.

Novel doped hydroxyapatite thin films obtained by pulsed laser deposition

International Nuclear Information System (INIS)

Duta, L.; Oktar, F.N.; Stan, G.E.; Popescu-Pelin, G.; Serban, N.; Luculescu, C.; Mihailescu, I.N.

2013-01-01

Highlights: ► HA coatings synthesized by pulsed laser deposition. ► Comparative study of commercial vs. animal origin materials. ► HA coatings of animal origin were rougher and more adherent to substrates. ► Animal origin films can be considered as promising candidates for implant coatings. - Abstract: We report on the synthesis of novel ovine and bovine derived hydroxyapatite thin films on titanium substrates by pulsed laser deposition for a new generation of implants. The calcination treatment applied to produce the hydroxyapatite powders from ovine/bovine bones was intended to induce crystallization and to prohibit the transmission of diseases. The deposited films were characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and energy dispersive X-ray spectroscopy. Pull-off adherence and profilometry measurements were also carried out. X-ray diffraction ascertained the polycrystalline hydroxyapatite nature of the powders and films. Fourier transform infrared spectroscopy evidenced the vibrational bands characteristic to a hydroxyapatite material slightly carbonated. The micrographs of the films showed a uniform distribution of spheroidal particulates with a mean diameter of ∼2 μm. Pull-off measurements demonstrated excellent bonding strength values between the hydroxyapatite films and the titanium substrates. Because of their physical–chemical properties and low cost fabrication from renewable resources, we think that these new coating materials could be considered as a prospective competitor to synthetic hydroxyapatite used for implantology applications.

Hydroxyapatite granules used in the obliteration of mastoid cavities in rats.

Science.gov (United States)

Hamerschmidt, Rogério; Santos, Rafael Francisco dos; Araújo, João Cândido; Stahlke, Henrique Jorge; Agulham, Miguel Angelo; Moreira, Ana Tereza Ramos; Mocellin, Marcos

2011-06-01

Prospective experimental study in which we created a bony defect in the mastoids of rats and filled it up with hydroxyapatite to evaluate bone regeneration, to solve the problems of open cavities after mastoidectomies that frequently present with otorrhea, infection, granulation tissue and hearing loss. The aim was to evaluate bone regeneration in defects created in the mastoids of rats, using hydroxyapatite, to see how much of the cavity we could reduce. Twelve rats Wistar-Furth were used. A 0.5 x 0.5 cm bone defect was created in both temporal bones of the rats, and filled with 15 micrograms of hydroxyapatite. The left side was used as control. The animals were slaughtered 40 days afterwards and histology analyses were carried out. In the hydroxyapatite group, the new bone growth involved an area of 68.53% of the total; and in the control group it was only of 15.97%. It was observed a very good hydroxyapatite integration to the temporal bone in this experimental model. The microscopic results were superior with the use of hydroxyapatite when compared to the control group. It is a safe method and easy to apply to solve the problems of open cavities with chronic discharge and difficult to clean.

Ostrich eggshell as an alternative raw material for hydroxyapatite synthesis

International Nuclear Information System (INIS)

Caliman, L.B.; Gouvea, D.

2011-01-01

The goal of this study was to investigate the use of ostrich eggshell for hydroxyapatite synthesis, a biomaterial of great medical importance due to its high biocompatibility. The eggshell was used as calcium ions source due its great containing of CaCO3. For its utilization, the eggshell was calcined and the obtained oxide (CaO) was transformed into Ca(OH)_2. Hydroxyapatite synthesis consisted in a wet precipitation reaction between Ca(OH)_2 and commercial H_3PO_4. The X ray Diffraction analysis has shown that the precipitated Hydroxyapatite calcined at 800°C resulted in a bifasic powder of Hydroxyapatite and β-Tricalcium Phosphate, which proves that this precipitated Hydroxyapatite was deficient in calcium. The Infrared Spectroscopy, showed the presence of CO_3"2"- ions, result of carrying out the reaction in open atmosphere. By Scanning Electron Microscopy nanometric particles arranged in agglomerates were observed and Specific Surface Area measurement resulted in 11,70 m²/g. Following this procedure, the ostrich eggshell gets a technological profitable reuse also environmentally friendly, being transformed in a new product of high aggregate value. (author)

Synthesis of nanocrystalline fluorinated hydroxyapatite

Indian Academy of Sciences (India)

Fluorinated hydroxyapatite; nanocrystalline; microwave synthesis; dissolution. ... HA by the presence of other ions such as carbonate, magnesium, fluoride, etc. ... Fourier transform infrared spectroscopy (FT–IR) and laser Raman spectroscopy.

Electrochemical properties of Ti3+ doped Ag-Ti nanotube arrays coated with hydroxyapatite

Science.gov (United States)

Zhang, Hangzhou; Shi, Xiaoguo; Tian, Ang; Wang, Li; Liu, Chuangwei

2018-04-01

Ag-Ti nanotube array was prepared by simple anodic oxidation method and uniform hydroxyapatite were electrochemically deposited on the nanotubes, and then characterized by SEM, XRD, XPS and EIS. In order to investigate the influence of Ti3+ on the electrochemical deposition of hydroxyapatite on the nanotubes, the Ag-Ti nanotube array self-doped with Ti3+ was prepared by one step reduction method. The experiment results revealed that the Ti3+ can promote the grow rate of hydroxyapatite coatings on nanotube surface. The hydroxyapatite coated Ag-Ti nanotube arrays with Ti3+ exhibit excellent stability and higher corrosion resistance. Moreover, the compact and dense hydroxyapatite coating can also prevent the Ag atom erosion from the Ag-Ti nanotube.

Crystalline and Crystalline International Disposal Activities

Energy Technology Data Exchange (ETDEWEB)

Viswanathan, Hari S. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Chu, Shaoping [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Dittrich, Timothy M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Hyman, Jeffrey De' Haven [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Karra, Satish [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Makedonska, Nataliia [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Reimus, Paul William [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2017-03-06

This report presents the results of work conducted between September 2015 and July 2016 at Los Alamos National Laboratory in the crystalline disposal and crystalline international disposal work packages of the Used Fuel Disposition Campaign (UFDC) for DOE-NE’s Fuel Cycle Research and Development program. Los Alamos focused on two main activities during this period: Discrete fracture network (DFN) modeling to describe flow and radionuclide transport in complex fracture networks that are typical of crystalline rock environments, and a comprehensive interpretation of three different colloid-facilitated radionuclide transport experiments conducted in a fractured granodiorite at the Grimsel Test Site in Switzerland between 2002 and 2013. Chapter 1 presents the results of the DFN work and is divided into three main sections: (1) we show results of our recent study on the correlation between fracture size and fracture transmissivity (2) we present an analysis and visualization prototype using the concept of a flow topology graph for characterization of discrete fracture networks, and (3) we describe the Crystalline International work in support of the Swedish Task Force. Chapter 2 presents interpretation of the colloidfacilitated radionuclide transport experiments in the crystalline rock at the Grimsel Test Site.

Ion exchange of strontium on synthetic hydroxyapatite

International Nuclear Information System (INIS)

Lazic, S.; Vukovic, Z.

1991-01-01

Adsorption of strontium ions on synthetic hydroxyapatite was examined using both batch and column methods. The apatite was prepared from aqueous solutions and characterized by standard analytical methods. The sample obtained had characteristics of well crystallized stoichiometric hydroxyapatite. The experimental data for sorption of strontium can be very well fitted with Langmuir's adsorption isotherm. It was found that sorption occurs by an ion exchange reaction between strontium ions in solution and calcium ions in apatite. (author) 14 refs.; 5 figs.; 1 tab

Hydroxyapatite based 99Mo-99mTc and 188W-188Re generator systems

International Nuclear Information System (INIS)

Monroy-Guzman, F.; Badillo-Almaraz, V.E.; Flores de la Torre, J.A.; Cosgrove, J.; Knapp, F.F. Jr.

2007-01-01

This paper describes studies evaluating the use of hydroxyapatite as the adsorbent material for both 90M o- 90m Tc and 89W - 188 Re generator systems. Hydroxyapatite is an insoluble solid with anion exchange properties. A study of the sorption behaviour of 90M o, 90m Tc, 188 W and 188 Re on hydroxyapatite in NaCl medium was evaluated by batch experiments. The results demonstrated that while 90M o, 90m Tc and 188 Re are not adsorbed by the hydroxyapatite in NaCl solutions (Kd 89W is strongly adsorbed (Kd >500). On the basis of these measurements, hydroxyapatite 89W - 188 Re generator systems were then constructed and eluted in NaCl solutions. The hydroxyapatite based 89W - 188 Re generator performances are presented. (author)

Hydroxyapatite does not improve the outcome of a bipolar hemiarthroplasty.

NARCIS (Netherlands)

Meijerink, H.J.; Gardeniers, J.W.M.; Buma, P.; Lemmens, J.A.M.; Schreurs, B.W.

2004-01-01

In a one-surgeon study the clinical and radiographic results of 30 cementless bipolar hip prostheses in 24 patients younger than 55 years were evaluated. Eleven noncoated prostheses (Noncoated Group) and 19 hydroxyapatite-coated prostheses (Hydroxyapatite Group) were compared after a mean followup

Nano Hydroxyapatite gel for removal of Nickel ions for environmental applications

International Nuclear Information System (INIS)

Abdelfattah, W.I.; Fayed, M.SH.; Gouda, SH.R.; Awwad, S.A.

2006-01-01

Hydroxyapatite (HAp) has been investigated for the removal of heavy metals in environmental application. However, little is known about the influences of surface modifications of the HAp. In the present study, nano HAp - polyvinyl alcohol gel was synthesized under ph control and the formed gel was used for removing nickel ions. The influence of nickel ions on the surface of HAp was studied. Reaction mechanisms were followed by ICP-MS and discussed via continuous variations method (CVM), mole ratio method (MRM) and slope ratio method (SRM). The formed gel with nickel ions was studied by various methods including UV, FTIR, XRD and SEM. The ICP-MS was used to analyze the supernatant solution to confirm the presence of Ca and / or Ni ions. The nickel ions were found to reduce the degree of crystallinity of the synthesized HAp phase. The present results indicated that nickel ions were completely adsorbed on the HAp structure with its anion. The validation of the nature of HAp gel as chelating agent or complex formation as well as physical sorption were discussed

Bioactive glass and hydroxyapatite thin films obtained by pulsed laser deposition

Energy Technology Data Exchange (ETDEWEB)

Gyorgy, E. [National Institute for Lasers, Plasma and Radiation Physics, P.O. Box MG 36, 77125 Bucharest (Romania) and Consejo Superior de Investigaciones Cientificas, Instituto de Ciencia de Materiales de Barcelona, Campus UAB, 08193 Bellaterra (Spain)]. E-mail: egyorgy@icmab.es; Grigorescu, S. [National Institute for Lasers, Plasma and Radiation Physics, P.O. Box MG 36, 77125 Bucharest (Romania); Socol, G. [National Institute for Lasers, Plasma and Radiation Physics, P.O. Box MG 36, 77125 Bucharest (Romania); Mihailescu, I.N. [National Institute for Lasers, Plasma and Radiation Physics, P.O. Box MG 36, 77125 Bucharest (Romania); Janackovic, D. [Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade (Serbia); Dindune, A. [Institute of Inorganic Chemistry of the Riga Technical University (Latvia); Plasma and Ceramic Technologies Ltd. (PCT Ltd.) (Latvia); Kanepe, Z. [Institute of Inorganic Chemistry of the Riga Technical University (Latvia); Plasma and Ceramic Technologies Ltd. (PCT Ltd.) (Latvia); Palcevskis, E. [Plasma and Ceramic Technologies Ltd. (PCT Ltd.) (Latvia); Zdrentu, E.L. [Institute of Biochemistry, Splaiul Independentei 296, Bucharest (Romania); Petrescu, S.M. [Institute of Biochemistry, Splaiul Independentei 296, Bucharest (Romania)

2007-07-31

Bioactive glass (BG), calcium hydroxyapatite (HA), and ZrO{sub 2} doped HA thin films were grown by pulsed laser deposition on Ti substrates. An UV KrF{sup *} ({lambda} = 248 nm, {tau} {>=} 7 ns) excimer laser was used for the multi-pulse irradiation of the targets. The substrates were kept at room temperature or heated during the film deposition at values within the (400-550 deg. C) range. The depositions were performed in oxygen and water vapor atmospheres, at pressure values in the range (5-40 Pa). The HA coatings were heat post-treated for 6 h in a flux of hot water vapors at the same temperature as applied during deposition. The surface morphology, chemical composition, and crystalline quality of the obtained thin films were studied by scanning electron microscopy, atomic force microscopy, and X-ray diffractometry. The films were seeded for in vitro tests with Hek293 (human embryonic kidney) cells that revealed a good adherence on the deposited layers. Biocompatibility tests showed that cell growth was better on HA than on BG thin films.

Synthesis of silver doped hydroxyapatite nanospheres using Ouzo effect

Directory of Open Access Journals (Sweden)

Marija Prekajski

2016-09-01

Full Text Available Nanoemulsion technique, based on Ouzo effect, was applied for synthesis of the pure and silver doped (2.5 and 5 mol% calcium hydroxyapatite (HAp. After calcination at 500 °C fully crystallized powders were obtained. X-ray powder diffraction analysis accompanied with Rietveld refinement revealed that the synthesized powders were single-phase hydroxyapatite. Raman spectroscopy also confirmed that the synthesized powders were single-phase. The obtained HAp particles were spherical in shape and their sizes were in the nanometer range which was revealed by field emission scanning electron microscopy analysis (FESEM. The successful synthesis of the single-phase Ag doped HAp showed that nanoemulsion method is a simple technique for obtaining pure and doped hydroxyapatite nanospheres.

Nanoparticle fabrication of hydroxyapatite by laser ablation in water

International Nuclear Information System (INIS)

Musaev, O. R.; Wieliczka, D. M.; Wrobel, J. M.; Kruger, M. B.; Dusevich, V.

2008-01-01

Synthetic polycrystalline hydroxyapatite was ablated in water with 337 nm radiation from a UV nitrogen pulsed laser. According to transmission electron microscopy micrographs, the ablated particles were approximately spherical and had a size of ∼80 nm. Raman spectroscopic analysis demonstrated that particles had the same structure as the original crystal. X-ray photoelectron spectroscopy showed that the surface chemical composition was close to that of the original material. The characteristics of the ablated particles and estimations of the temperature rise of the hydroxyapatite surface under laser irradiation are consistent with the mechanism of explosive boiling being responsible for ablation. The experimental observations offer the basis for preparation of hydroxyapatite nanoparticles by laser ablation in water

A graded graphene oxide-hydroxyapatite/silk fibroin biomimetic scaffold for bone tissue engineering.

Science.gov (United States)

Wang, Qian; Chu, Yanyan; He, Jianxin; Shao, Weili; Zhou, Yuman; Qi, Kun; Wang, Lidan; Cui, Shizhong

2017-11-01

To better mimic natural bone, a graphene oxide-hydroxyapatite/silk fibroin (cGO-HA/SF) scaffold was fabricated by biomineralizing carboxylated GO sheets, blending with SF, and freeze-drying. The material has increasing porosity and decreasing density from outside to inside. Analysis of GO mineralization in simulated body fluid indicated that carboxylation and Chitosan may synergistically regulate HA growth along the c-axis of weakly crystalline, rod-like GO-HA particles. Compared with HA/SF gradient composites, a cGO-HA gradient scaffold with cGO:HA mass ratio 1:4 has 5-fold and 2.5-fold higher compressive strength and compressive modulus, respectively. Additionally, the cGO-HA/SF composite stimulated mouse mesenchymal stem cell adhesion and proliferation, alkaline phosphatase secretion, and mineral deposition more strongly than HA/SF and pure HA scaffolds. Hence, the material may prove to be an excellent and versatile scaffold for bone tissue engineering. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of carbon nanotubes reinforced hydroxyapatite composite coatings on titanium by electrodeposition method

International Nuclear Information System (INIS)

Gopi, D.; Shinyjoy, E.; Sekar, M.; Surendiran, M.; Kavitha, L.; Sampath Kumar, T.S.

2013-01-01

Highlights: •Successful development of CNTs reinforced HAP coating on Ti by electrodeposition. •CNTs as a reinforcing material imparts strength and toughness to HAP. •Incorporating CNTs improves crystallinity, morphology, biological properties of HAP. •CNTs–HAP coating on Ti is bioresistive, better candidate for implant applications. -- Abstract: Carbon nanotubes (CNTs) are outstanding reinforcement material for imparting strength and toughness to brittle hydroxyapatite (HAP). This work reports the electrodeposition of CNTs reinforced HAP on titanium substrate at −1.4 V vs. SCE during 30 min with the functionalised CNTs concentration ranging from 0 to 2 wt.%. Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) equipped with energy dispersive X-ray analysis (EDX), high resolution transmission electron microscopy (HRTEM), mechanical and biological studies were used to characterise the coatings. Also, the corrosion resistance of the coatings was evaluated by electrochemical techniques in simulated body fluid (SBF) solution

Application of fluoridated hydroxyapatite thin film coatings using KrF pulsed laser deposition.

Science.gov (United States)

Hashimoto, Yoshiya; Ueda, Mamoru; Kohiga, Yu; Imura, Kazuki; Hontsu, Shigeki

2018-06-08

Fluoridated hydroxyapatite (FHA) was investigated for application as an implant coating for titanium bone substitute materials in dental implants. A KrF pulsed excimer deposition technique was used for film preparation on a titanium plate. The compacts were ablated by laser irradiation at an energy density of 1 J/cm 2 on an area 1×1 mm 2 with the substrate at room temparature. Energydispersive spectrometric analysis of the FHA film revealed peaks of fluorine in addition to calcium and phosphorus. X-ray diffraction revealed the presence of crystalline FHA on the FHA film after a 10 h post annealing treatment at 450°C. The FHA film coating exhibited significant dissolution resistance to sodium phosphate buffer for up to 21 days, and favorable cell attachment of human mesenchymal stem cells compared with HA film. The results of this study suggest that FHA coatings are suitable for real-world implantation applications.

Cytotoxicity of nano-hydroxyapatite on human-derived oral epithelium cell line: an in vitro study

Directory of Open Access Journals (Sweden)

Farid Abassi

2016-08-01

Full Text Available Background: Hydroxyapatite nanoparticles have a more surface contact and solubility than conventional hydroxyapatite. Hydroxynanoparticles enhances the biological and mechanical properties of new regenerated tissues. The hydroxyapatite nanoparticles have received attention as a new and effective osseous graft for using as scaffolds in bone regeneration. The reports on hydroxyapatite nanoparticles biocompatibility are controversial. It has been shown that hydroxyapatite nanoparticles induces inflammatory reaction and apoptosis. The aim of the present study was to evaluate the cytotoxicity of nano-hydroxyapatite on the human epithelial cells. Methods: The study was experimental and completed in vitro. The study was carried out in department of Immonulogy, Faculty of Medicine, Shahid Beheshti University of Medical Sciences in November 2014. The human-derived oral epithelium cell line (KB obtained from Pasteur Institute, Tehran, Iran were exposed to hydroxyapatite nanoparticles at 0.01, 0.05, 0.1, 0.5, 0.75, 1, 2.5 and 5 mg/ml concentrations in 24, 48 and 72 hours. Rod-shaped hydroxyapatite nanoparticles with 99% purity and maximum 100 nm sized particles were used. Methylthiazol tetrazolium bromide (MTT method was employed for cell vitality evaluation. Enzyme-linked immunosorbent assay (ELISA was used for assessing the viability of cells. Distilled water and fetal bovine serum (FBS were positive and negative controls. ANOVA and Duncan tests were used for statistical analysis. Results: The cytotoxicity of different concentrations of hydroxyapatite nanoparticles on human-derived oral epithelium cell line in 24 (P< 0.001, 48 (P< 0.001 and 72 hours (P< 0.001 was significantly different. The nano-hydroxyapatite particles at 0.5 to 1 mg/ml had the highest cytotoxicity effect on human-derived oral epithelium cells in 24, 48 and 72 hours. Lower concentrations than 0.05 mg/ml had the best biocompatibility properties in 24, 48 and 72 hours. Conclusion

Tungsten carbide-cobalt as a nanoparticulate reference positive control in in vitro genotoxicity assays.

Science.gov (United States)

Moche, Hélène; Chevalier, Dany; Barois, Nicolas; Lorge, Elisabeth; Claude, Nancy; Nesslany, Fabrice

2014-01-01

With the increasing human exposure to nanoparticles (NP), the evaluation of their genotoxic potential is of significant importance. However, relevance for NP of the routinely used in vitro genotoxicity assays is often questioned, and a nanoparticulate reference positive control would therefore constitute an important step to a better testing of NP, ensuring that test systems are really appropriate. In this study, we investigated the possibility of using tungsten carbide-cobalt (WC-Co) NP as reference positive control in in vitro genotoxicity assays, including 2 regulatory assays, the mouse lymphoma assay and the micronucleus assay, and in the Comet assay, recommended for the toxicological evaluation of nanomedicines by the French Agency of Human Health Products (Afssaps). Through these assays, we were able to study different genetic endpoints in 2 cell types commonly used in regulatory genotoxicity assays: the L5178Y mouse lymphoma cell line and primary cultures of human lymphocytes. Our results showed that the use of WC-Co NP as positive control in in vitro genotoxicity assays was conceivable, but that different parameters have to be considered, such as cell type and treatment schedule. L5178Y mouse lymphoma cells did not provide satisfactory results in the 3 performed tests. However, human lymphocytes were more sensitive to genotoxic effects induced by WC-Co NP, particularly after a 24-h treatment in the in vitro micronucleus assay and after a 4-h treatment in the in vitro Comet assay. Under such conditions, WC-Co could be used as a nanoparticulate reference positive control in these assays.

Study on removal effect and mechanism of uranium by hydroxyapatite and natural apatite

International Nuclear Information System (INIS)

Zhang Xiaofeng; Chen Diyun; Tu Guoqing; Huang Xiaozhui

2014-01-01

By the static experiments, the effects of reaction time, pH value, initial concentration of uranium, dosage of apatite on adsorption of hydroxyapatite and natural apatite for uranium were studied respectively. The adsorption process was analyzed by thermodynamics and kinetics, and the adsorption mechanism was analyzed by infrared spectroscopy, X-ray diffraction and scanning electron microscope. The results of hydroxyapatite show that the removal capacity of uranium increases with the initial concentration of uranium, and the adsorption rate of hydroxyapatite on UO_2"2"+ reaches 85%, when the pH value is 4 to 5 and dosage of hydroxyapatite is 0.75 g. The results of natural apatite show that the removal capacity of uranium increases with the initial concentration of uranium, and the adsorption rate of natural apatite on UO_2"2"+ is up to 80%, when the pH value is 3 and dosage of hydroxyapatite is l.0 g. Similarly, at 120 minutes both of the removal reactions by hydroxyapatite and natural apatite substantially reach equilibrium. Moreover, both of the reactions by hydroxyapatite and natural apatite are in line with quasi secondary dynamics equation, and follow the Langmuir adsorption isotherm. Infrared spectra indicate that the removal of hydroxyapatite for uranium depends on the complexation of phosphate, which is almost the same as that of natural apatite. X-ray diffraction analysis shows that hydroxyapatite has the composition and structure of pure material, whereas the natural apatite is mainly composed of Ca_5H_2(PO_4)_3F and Ca_8H_2(PO_4)_6H_2O. In addition, scanning electron microscope demonstrates that hydroxyapatite has the appearance of spherical with a hole and the hole has a cavity containing a large amount of floc, while the surface becomes smooth and pores are closed after removal of uranium, which is due to the adsorption of UO_2"2"+ leading a link between molecules on hydroxyapatite surface. But for natural apatite, it depicts the angular mineral shape

Biomorphous porous hydroxyapatite-ceramics from rattan (Calamus Rotang).

Science.gov (United States)

Eichenseer, Christiane; Will, Julia; Rampf, Markus; Wend, Süsen; Greil, Peter

2010-01-01

The three-dimensional, highly oriented pore channel anatomy of native rattan (Calamus rotang) was used as a template to fabricate biomorphous hydroxyapatite (Ca(5)(PO(4))(3)OH) ceramics designed for bone regeneration scaffolds. A low viscous hydroxyapatite-sol was prepared from triethyl phosphite and calcium nitrate tetrahydrate and repeatedly vacuum infiltrated into the native template. The template was subsequently pyrolysed at 800 degrees C to form a biocarbon replica of the native tissue. Heat treatment at 1,300 degrees C in air atmosphere caused oxidation of the carbon skeleton and sintering of the hydroxyapatite. SEM analysis confirmed detailed replication of rattan anatomy. Porosity of the samples measured by mercury porosimetry showed a multimodal pore size distribution in the range of 300 nm to 300 microm. Phase composition was determined by XRD and FT-IR revealing hydroxyapatite as the dominant phase with minimum fractions of CaO and Ca(3)(PO(4))(2). The biomorphous scaffolds with a total porosity of 70-80% obtained a compressive strength of 3-5 MPa in axial direction and 1-2 MPa in radial direction of the pore channel orientation. Bending strength was determined in a coaxial double ring test resulting in a maximum bending strength of approximately 2 MPa.

Investigation of the interaction of hydroxyapatite with technetium in association with stannous pyrophosphate

International Nuclear Information System (INIS)

Billinghurst, M.W.; Jette, D.; Somers, E.

1981-01-01

The individual components of technetium-99m stannous pyrophosphate were studied with respect to their interaction with hydroxyapatite. It is demonstrated that the role of the pyrophosphate molecule is one of a solubilizing and transporting molecule to carry the technetium atom to the site of the hydroxyapatite where the chelate disassociates and both the pyrophosphate and the technetium individually bind to the hydroxyapatite. The stannous ion is shown to associate with the hydroxyapatite also and although also solubilized by the pyrophosphate appears to be less strongly associated with the pyrophosphate. (author)

The electrolysis time on electrosynthesis of hydroxyapatite with bipolar membrane

Science.gov (United States)

Nur, Adrian; Jumari, Arif; Budiman, Anatta Wahyu; Puspitaningtyas, Stella Febianti; Cahyaningrum, Suci; Nazriati, Nazriati; Fajaroh, Fauziatul

2018-02-01

The electrochemical method with bipolar membrane has been successfully used for the synthesis of hydroxyapatite. In this work, we have developed 2 chambers electrolysis system separated by a bipolar membrane. The membrane was used to separate cations (H+ ions produced by the oxidation of water at the anode) and anions (OH- ions produced by the reduction of water at the cathode). With this system, we have designed that OH- ions still stay in the anions chamber because OH- ions was very substantial in the hydroxyapatite particles formation. The aim of this paper was to compare the electrolysis time on electrosynthesis of hydroxyapatite with and without the bipolar membrane. The electrosynthesis was performed at 500 mA/cm2 for 0.5 to 2 hours at room temperature and under ultrasonic cleaner to void agglomeration with and without the bipolar membrane. The electrosynthesis of hydroxyapatite with the bipolar membrane more effective than without the bipolar membrane. The hydroxyapatite has been appeared at 0.5 h of the electrolysis time with the bipolar membrane (at the cathode chamber) while it hasn't been seen without the bipolar membrane. The bipolar membrane prevents OH- ions migrate to the cation chamber. The formation of HA becomes more effective because OH- ions just formed HA particle.

Crystalline and Crystalline International Disposal Activities

Energy Technology Data Exchange (ETDEWEB)

Viswanathan, Hari S. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Chu, Shaoping [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Reimus, Paul William [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Makedonska, Nataliia [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Hyman, Jeffrey De' Haven [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Karra, Satish [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Dittrich, Timothy M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

2015-12-21

This report presents the results of work conducted between September 2014 and July 2015 at Los Alamos National Laboratory in the crystalline disposal and crystalline international disposal work packages of the Used Fuel Disposition Campaign (UFDC) for DOE-NE’s Fuel Cycle Research and Development program.

In vitro mechanical integrity of hydroxyapatite coated magnesium alloy

International Nuclear Information System (INIS)

Kannan, M Bobby; Orr, Lynnley

2011-01-01

The mechanical integrity of resorbable implants during service, especially in load bearing orthopaedic applications, is critical. The high degradation rate of resorbable magnesium and magnesium-based implants in body fluid may potentially cause premature in-service failure. In this study, a magnesium alloy (AZ91) was potentiostatically coated with hydroxyapatite at different cathodic voltages in an attempt to enhance the mechanical integrity. The mechanical integrity of the uncoated and hydroxyapatite coated alloys was evaluated after in vitro testing of the coated samples in simulated body fluid (SBF). The uncoated alloy showed 40% loss in the mechanical strength after five days exposure to SBF. However, the hydroxyapatite coated alloy exposed to SBF showed 20% improvement in the mechanical strength as compared to that of the uncoated alloy. The alloy coated potentiostatically at -2 V performed better than the -3 V coated alloy. The cross-sectional analysis of the coatings revealed relatively uniform coating thickness for the -2 V coated alloy, whereas the -3 V coated alloy exhibited areas of uneven coating. This can be attributed to the increase in hydrogen evolution on the alloy during -3 V coating as compared to -2 V coating. The scanning electron micrographs of the in vitro tested alloy revealed that hydroxyapatite coating significantly reduced the localized corrosion of the alloy, which is critical for better in-service mechanical integrity. Thus, the study suggests that the in vitro mechanical integrity of resorbable magnesium-based alloy can be improved by potentiostatic hydroxyapatite coating.

In vitro mechanical integrity of hydroxyapatite coated magnesium alloy

Energy Technology Data Exchange (ETDEWEB)

Kannan, M Bobby; Orr, Lynnley, E-mail: bobby.mathan@jcu.edu.au [Discipline of Chemical Engineering, School of Engineering and Physical Sciences, James Cook University, Townsville, Queensland 4811 (Australia)

2011-08-15

The mechanical integrity of resorbable implants during service, especially in load bearing orthopaedic applications, is critical. The high degradation rate of resorbable magnesium and magnesium-based implants in body fluid may potentially cause premature in-service failure. In this study, a magnesium alloy (AZ91) was potentiostatically coated with hydroxyapatite at different cathodic voltages in an attempt to enhance the mechanical integrity. The mechanical integrity of the uncoated and hydroxyapatite coated alloys was evaluated after in vitro testing of the coated samples in simulated body fluid (SBF). The uncoated alloy showed 40% loss in the mechanical strength after five days exposure to SBF. However, the hydroxyapatite coated alloy exposed to SBF showed 20% improvement in the mechanical strength as compared to that of the uncoated alloy. The alloy coated potentiostatically at -2 V performed better than the -3 V coated alloy. The cross-sectional analysis of the coatings revealed relatively uniform coating thickness for the -2 V coated alloy, whereas the -3 V coated alloy exhibited areas of uneven coating. This can be attributed to the increase in hydrogen evolution on the alloy during -3 V coating as compared to -2 V coating. The scanning electron micrographs of the in vitro tested alloy revealed that hydroxyapatite coating significantly reduced the localized corrosion of the alloy, which is critical for better in-service mechanical integrity. Thus, the study suggests that the in vitro mechanical integrity of resorbable magnesium-based alloy can be improved by potentiostatic hydroxyapatite coating.

Effect of nano-hydroxyapatite concentration on remineralization of initial enamel lesion in vitro

International Nuclear Information System (INIS)

Huang, S B; Gao, S S; Yu, H Y

2009-01-01

The purpose of the research was to determine the effect of nano-hydroxyapatite concentrations on initial enamel lesions under dynamic pH-cycling conditions. Initial enamel lesions were prepared in bovine enamel with an acidic buffer. NaF (positive control), deionized water (negative control) and four different concentrations of nano-hydroxyapatite (1%, 5%, 10% and 15% wt%) were selected as the treatment agents. Surface microhardness (SMH) measurements were performed before/after demineralization and after 3, 6, 9 and 12 days of application, and the percentage surface microhardness recovery (%SMHR) was calculated. The specimens were then examined by a scanning electron microscope. The %SMHR in nano-hydroxyapatite groups was significantly greater than that of negative control. When the concentration of nano-HA was under 10%, SMH and %SMHR increased with increasing nano-hydroxyapatite concentrations. There were no significant differences between the 10% and 15% groups at different time periods in the pH-cycling. The SEM analysis showed that nano-hydroxyapatite particles were regularly deposited on the cellular structure of the demineralized enamel surface, which appeared to form new surface layers. It was concluded that nano-hydroxyapatite had the potential to remineralize initial enamel lesions. A concentration of 10% nano-hydroxyapatite may be optimal for remineralization of early enamel caries.

Effect of nano-hydroxyapatite concentration on remineralization of initial enamel lesion in vitro

Energy Technology Data Exchange (ETDEWEB)

Huang, S B; Gao, S S; Yu, H Y, E-mail: yhyang6812@scu.edu.c [State Key Laboratory of Oral Diseases, West China Hospital of Stomatology, Sichuan University, Chengdu 610041 (China)

2009-06-15

The purpose of the research was to determine the effect of nano-hydroxyapatite concentrations on initial enamel lesions under dynamic pH-cycling conditions. Initial enamel lesions were prepared in bovine enamel with an acidic buffer. NaF (positive control), deionized water (negative control) and four different concentrations of nano-hydroxyapatite (1%, 5%, 10% and 15% wt%) were selected as the treatment agents. Surface microhardness (SMH) measurements were performed before/after demineralization and after 3, 6, 9 and 12 days of application, and the percentage surface microhardness recovery (%SMHR) was calculated. The specimens were then examined by a scanning electron microscope. The %SMHR in nano-hydroxyapatite groups was significantly greater than that of negative control. When the concentration of nano-HA was under 10%, SMH and %SMHR increased with increasing nano-hydroxyapatite concentrations. There were no significant differences between the 10% and 15% groups at different time periods in the pH-cycling. The SEM analysis showed that nano-hydroxyapatite particles were regularly deposited on the cellular structure of the demineralized enamel surface, which appeared to form new surface layers. It was concluded that nano-hydroxyapatite had the potential to remineralize initial enamel lesions. A concentration of 10% nano-hydroxyapatite may be optimal for remineralization of early enamel caries.

Towards the synthesis of hydroxyapatite/protein scaffolds with controlled porosities: bulk and interfacial shear rheology of a hydroxyapatite suspension with protein additives.

Science.gov (United States)

Maas, Michael; Bodnar, Pedro Marcus; Hess, Ulrike; Treccani, Laura; Rezwan, Kurosch

2013-10-01

The synthesis of porous hydroxyapatite scaffolds is essential for biomedical applications such as bone tissue engineering and replacement. One way to induce macroporosity, which is needed to support bone in-growth, is to use protein additives as foaming agents. Another reason to use protein additives is the potential to introduce a specific biofunctionality to the synthesized scaffolds. In this work, we study the rheological properties of a hydroxyapatite suspension system with additions of the proteins bovine serum albumin (BSA), lysozyme (LSZ) and fibrinogen (FIB). Both the rheology of the bulk phase as well as the interfacial shear rheology are studied. The bulk rheological data provides important information on the setting behavior of the thixotropic suspension, which we find to be faster with the addition of FIB and LSZ and much slower with BSA. Foam bubble stabilization mechanisms can be rationalized via interfacial shear rheology and we show that it depends on the growth of interfacial films at the suspension/air interface. These interfacial films support the stabilization of bubbles within the ceramic matrix and thereby introduce macropores. Due to the weak interaction of the protein molecules with the hydroxyapatite particles of the suspension, we find that BSA forms the most stable interfacial films, followed by FIB. LSZ strongly interacts with the hydroxyapatite particles and thus only forms thin films with very low elastic moduli. In summary, our study provides fundamental rheological insights which are essential for tailoring hydroxyapatite/protein suspensions in order to synthesize scaffolds with controlled porosities. Copyright © 2013 Elsevier Inc. All rights reserved.

Fabrication of hydroxyapatite from fish bones waste using reflux method

Science.gov (United States)

Cahyanto, A.; Kosasih, E.; Aripin, D.; Hasratiningsih, Z.

2017-02-01

The aim of this present study was to investigate the fabrication of hydroxyapatites, which were synthesized from fish bone wastes using reflux method. The fish bone wastes collected from the restaurant were brushed and boiled at 100°C for 10 minutes to remove debris and fat. After drying, the fish bones were crushed, and ball milled into a fine powder. The fish bone wastes were then processed by refluxing using KOH and H3PO4 solutions. The samples were calcined at 900°C and characterized by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectrometry (FT-IR). The XRD pattern of samples after treatment revealed that the peak of hydroxyapatite was observed and the bands of OH- and PO4 3- were observed by FT-IR. The scanning electron microscope evaluation of sample showed the entangled crystal and porous structure of hydroxyapatite. In conclusion, the hydroxyapatite was successfully synthesized from fish bone wastes using reflux method.

Vesicular delivery of crystalline calcium minerals to ECM in biomineralized nanoclay composites

International Nuclear Information System (INIS)

Katti, Kalpana S; Ambre, Avinash H; Payne, Scott; Katti, Dinesh R

2015-01-01

The mechanisms of mineralization and new bone formation were explored in newly formed extracellular matrix in a nanoclay based composite. Nanoclay films were prepared by intercalating the clays with amino acids and using the amino acids for mineralization of hydroxyapatite. The biomineralized hydroxyapatite (HAP) inside nanoclay galleries or in situ HAP/clay was further used to make films (substrates) using polycaprolactone (PCL) that were seeded with mesenchymal stem cells in a two-stage seeding process. SEM imaging experiments performed on PCL/in situ HAPclay composite films seeded with human MSCs indicated formation of matrix vesicles. The vesicles appear to emerge from the cells that are adhered to the nanoclay HAP films and also deposited in the extracellular space. Vesicles are also observed to be embedded in the cells or under the surface of cells. Crystalline structures with Ca and P were found inside vesicles. The Ca/P ratios obtained using energy dispersive spectroscopy indicate values ranging from below 0.7 to the stoichiometric HAP value of 1.67. The Ca/P ratios were obtained to be closer to the stoichiometric value for single seeding experiments as compared to the double seeding experiments indicating more new bone formation in double seeding experiments. New bone formation with bone mimetic mineralization is thus observed on the in situ HAP nanoclay PCL samples. Hence the PCL/in situ HAPclay composites besides being osteoinductive are also capable of providing a favorable micro-environment for cell dependent processes involved in bone mineral formation. (paper)

Mechanical properties of hydroxyapatite single crystals from nanoindentation data

Science.gov (United States)

Zamiri, A.; De, S.

2011-01-01

In this paper we compute elasto-plastic properties of hydroxyapatite single crystals from nanindentation data using a two-step algorithm. In the first step the yield stress is obtained using hardness and Young’s modulus data, followed by the computation of the flow parameters. The computational approach is first validated with data from existing literature. It is observed that hydroxyapatite single crystals exhibit anisotropic mechanical response with a lower yield stress along the [1010] crystallographic direction compared to the [0001] direction. Both work hardening rate and work hardening exponent are found to be higher for indentation along the [0001] crystallographic direction. The stress-strain curves extracted here could be used for developing constitutive models for hydroxyapatite single crystals. PMID:21262492

Different properties exhibited on the two typical crystal faces of hydroxyapatite in a simulated body environment

Energy Technology Data Exchange (ETDEWEB)

Hagio, T; Iwai, K [Department of Materials, Physics and Energy Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya, 464-8603 (Japan); Tanase, T [Toho Gas Corporation, 19-18 Sakurada-cho, Atsuta-ku, Nagoya, 456-8511 (Japan); Akiyama, J [Institute for Molecular Science, National Institute of Natural Sciences, 38 Nishigonaka, Myodaiji, Okazaki, 444-8585 (Japan); Asai, S [Innovation Plaza Tokai Japan Science and Technology Agency, 23-1 Ahara-cho, Minami-ku, Nagoya, 457-0063 (Japan)], E-mail: hagio.takeshi@h.mbox.nagoya-u.ac.jp

2009-03-01

Hydroxyapatite is a main mineral constituent of hard tissues and is extensively used as a biomaterial in the medical field. Hydroxyapatite exhibits anisotropic chemical properties on its two typical crystal faces, the a-face and c-face, due to its hexagonal crystal structure. In polycrystalline bodies, such anisotropy can be enhanced by controlling the crystal orientation. Hydroxyapatite nanocrystals that constitute long bones also form a crystal oriented structure. Therefore, clarification of the difference between the properties of a-face and c-face in hydroxyapatite using in vitro experiments is useful to understand the structure and function of actual hard tissues. Hydroxyapatite ceramics with controlled crystal orientation were prepared by a slip casting method under application of a magnetic field. The fabricated hydroxyapatite ceramics had surfaces consisting mainly of a-face, or otherwise c-face hydroxyapatite. These hydroxyapatite ceramics were immersed into simulated body fluids to investigate the difference in bioactivity. The precipitation behavior observed on the surface of each hydroxyapatite ceramic was different. The thickness of the precipitate was increased and formed earlier on the HAp c-face compared to that on the a-face.

Different properties exhibited on the two typical crystal faces of hydroxyapatite in a simulated body environment

International Nuclear Information System (INIS)

Hagio, T; Iwai, K; Tanase, T; Akiyama, J; Asai, S

2009-01-01

Hydroxyapatite is a main mineral constituent of hard tissues and is extensively used as a biomaterial in the medical field. Hydroxyapatite exhibits anisotropic chemical properties on its two typical crystal faces, the a-face and c-face, due to its hexagonal crystal structure. In polycrystalline bodies, such anisotropy can be enhanced by controlling the crystal orientation. Hydroxyapatite nanocrystals that constitute long bones also form a crystal oriented structure. Therefore, clarification of the difference between the properties of a-face and c-face in hydroxyapatite using in vitro experiments is useful to understand the structure and function of actual hard tissues. Hydroxyapatite ceramics with controlled crystal orientation were prepared by a slip casting method under application of a magnetic field. The fabricated hydroxyapatite ceramics had surfaces consisting mainly of a-face, or otherwise c-face hydroxyapatite. These hydroxyapatite ceramics were immersed into simulated body fluids to investigate the difference in bioactivity. The precipitation behavior observed on the surface of each hydroxyapatite ceramic was different. The thickness of the precipitate was increased and formed earlier on the HAp c-face compared to that on the a-face.

Production and analysis of hydroxyapatite from Australian corals via hydrothermal process

International Nuclear Information System (INIS)

Hu, J.; Russell, J.; Ben-Nissan, B.

1999-01-01

Since the 1970s it is well known that if a biocompatible ceramic prosthesis with appropriate interconnected pores is used, growth of hard and soft tissue into the surface pores will be observed. A very strong attachment and hence the resultant mechanical and chemical bond to the existing surrounding tissue will be produced. Current artificial eyes although widely used encounter various problems due to the their motility and fail to deliver natural movement. They also cause sagging of the lids due to unsupported weight of the prosthesis. It is expected that application of a porous bioceramic such as the hydroxyapatite can generate good bonding to the tissue and hence a life-like eye movement. Hydroxyapatite (HAp) and related calcium phosphates have been studied for many years as implant materials, due to their similarity with the mineral phase of bone. From the point of view of biocompatibility, HAp seems to be the most suitable ceramic material for tissue replacement implants. Hydroxyapatite ceramics do not exhibit any cytoxic effects. It shows excellent biocompatibility with hard and soft tissues. Moreover, HAp can directly bond to the bone. Various preparation methods for HAp including the hydrothermal method have been used. The hydrothermal method was first used for hydroxyapatite formation directly from corals in 1974 by Roy and Linnehan. Complete replacement of aragonite by phosphatic material was achieved under 270degC and 103MPa using the hydrothermal process. This process has the disadvantage that the hydrothermal treatment must be carried out at a relatively high temperature under very high pressure. In 1996, HAp derived from Indian coral using hydrothermal process was developed by Sivakumar et al. However, the resultant material was in the form of a powder. Australia has rich variety of corals. Their application for implants have been studied very little. In this study, Australian corals selected were used for hydroxyapatite conversion. A new hydrothermal

In vitro and in vivo evaluation of silicated hydroxyapatite and impact of insulin adsorption.

Science.gov (United States)

Lasgorceix, M; Costa, A M; Mavropoulos, E; Sader, M; Calasans, M; Tanaka, M N; Rossi, A; Damia, C; Chotard-Ghodsnia, R; Champion, E

2014-10-01

This study evaluates the biological behaviour, in vitro and in vivo, of silicated hydroxyapatite with and without insulin adsorbed on the material surface. Insulin was successfully adsorbed on hydroxyapatite and silicated hydroxyapatite bioceramics. The modification of the protein secondary structure after the adsorption was investigated by means of infrared and circular dichroism spectroscopic methods. Both results were in agreement and indicated that the adsorption process was likely to change the secondary structure of the insulin from a majority of α-helix to a β-sheet form. The biocompatibility of both materials, with and without adsorbed insulin on their surface, was demonstrated in vitro by indirect and direct assays. A good viability of the cells was found and no proliferation effect was observed regardless of the material composition and of the presence or absence of insulin. Dense granules of each material were implanted subcutaneously in mice for 1, 3 and 9 weeks. At 9 weeks of implantation, a higher inflammatory response was observed for silicated hydroxyapatite than for pure hydroxyapatite but no significant effect of adsorbed insulin was detected. Though the presence of silicon in hydroxyapatite did not improve the biological behaviour, the silicon substituted hydroxyapatite remained highly viable.

Mechanical response and multilevel structure of biomimetic hydroxyapatite/polygalacturonic/chitosan nanocomposites

International Nuclear Information System (INIS)

Verma, Devendra; Katti, Kalpana S.; Katti, Dinesh R.; Mohanty, Bedabibhas

2008-01-01

Using an in situ mineralization process that is biomimetic we have synthesized new nanocomposites of chitosan/hydroxyapatite in 50-50 ratio(ChiHAP50), polygalacturonic acid/hydroxyapatite in 50-50 ratio (PgAHAP50) and Chitosan/hydroxyapatite/Polygalacturonic acid (ChiPgAHAP50). Polygalacturonic acid (PgA) is electrostatically complementary to chitosan, and thus is expected to provide stronger interfacial interactions and improve mechanical response. Atomic force imaging of fractured and polished surfaces suggests a multilevel organization in the hydroxyapatite/biopolymer nanocomposite. The AFM images of ChiPgAHAP50 nanocomposite display presence of chitosan rich and polygalacturonic rich domains. These chitosan rich and PgA rich domains are made of smaller globular shaped particles in which, hydroxyapatite nano-particles are embedded in the biopolymer matrix. The average size of the hydroxyapatite particles in PgAHAP50, ChiHAP50 and ChiPgAHAP50 were found to be 25, 42 and 34 nm respectively. The elastic moduli determined from nanoindentation of PgAHAP50, ChiHAP50 and ChiPgAHAP50 composites are 29.81, 17.56 and 23.62 GPa respectively. Hardness values of the three composites in the same order were found to be 1.56, 0.65 and 1.14 GPa respectively. Macro-mechanical tests showed significant enhancement in elastic moduli, strain to failure and compressive strength of ChiPgAHAP50 composites over ChiHAP50 and PgAHAP50

Sorption of U(VI) species on hydroxyapatite

International Nuclear Information System (INIS)

Thakur, P.; Moore, R.C.; Choppin, G.R.

2005-01-01

The sorption of uranyl (UO 2 2+ ) cations to hydroxyapatite was studied as a function of the amount of sorbent, ionic strength, U(VI) concentration, pH and temperature. The rate of uranyl sorption on hydroxyapatite decreased with increased uranyl concentrations. The amount sorbed decreased with increased ionic strength and increased with pH to a maximum at 7-8. The sorption data for UO 2 2+ were fitted well by the Freundlich and Dubinin-Radushkevich (D-R) isotherms. The anions Cl - , NO 3 - , SO 4 2- and CH 3 COO - decreased the sorption of uranium on hydroxyapatite while S 2 O 3 2- slightly increased it. The sorbed uranium was desorbed by 0.10 M and 1.00 M solutions of HCl and HNO 3 . The thermodynamic parameters for the sorption of UO 2 2+ were measured at temperatures of 298, 313, 323 and 333 K. The temperature dependence confirmed an endothermic heat of sorption. The activation energy for the sorption process was calculated to be +2.75±0.02 kJ/mol. (orig.)

Biomimetic synthesis of hydroxyapatite/bacterial cellulose nanocomposites for biomedical applications

International Nuclear Information System (INIS)

Wan, Y.Z.; Huang, Y.; Yuan, C.D.; Raman, S.; Zhu, Y.; Jiang, H.J.; He, F.; Gao, C.

2007-01-01

Hydroxyapatite (HAp) and bacterial cellulose (BC) are both excellent materials for use in biomaterial areas. The former has outstanding osteoconductivity and bioactivity and the latter is a high-strength nano-fibrous and extensively used biomaterial. In this work, the HAp/BC nanocomposites with a 3-dimensional (3-D) network were synthesized via a biological route by soaking both phosphorylated and unphosphorylated BCs in 1.5 simulated body fluid (SBF). Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), and transmission electron microscopy (TEM) were employed to characterize the HAp/BC nanocomposites. SEM observations demonstrated that HAp crystals were uniformly formed on the phosphorylated BC fibers after soaking in 1.5 SBF whereas little HAp was observed on individual unphosphorylated BC fibers. Our experimental results suggested that the unphosphorylated BC did not induce HAp growth and that phosphorylation effectively triggered HAp formation on BC. Mechanisms were proposed for the explanation of the experimental observations. XRD and FTIR results revealed that the HAp crystals formed on the phosphorylated BC fibers were carbonate-containing with nano-sized crystallites and crystallinities less than 1%. These structural features were close to those of biological apatites

Biomimetic synthesis of hydroxyapatite/bacterial cellulose nanocomposites for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Wan, Y.Z. [School of Materials Science and Engineering, Tianjin University, Tianjin 300072 (China)]. E-mail: yzwantju@yahoo.com; Huang, Y. [School of Materials Science and Engineering, Tianjin University, Tianjin 300072 (China); Yuan, C.D. [School of Chemical Engineering, Tianjin University, Tianjin 300072 (China); Raman, S. [Department of Community Health and Epidemiology, Queen' s University, Kingston, Ontario, Canada K7L 3N6 (Canada); Zhu, Y. [School of Chemical Engineering, Tianjin University, Tianjin 300072 (China); Jiang, H.J. [Wendeng Hospital of Orthopaedics, Shandong 264400 (China); He, F. [School of Materials Science and Engineering, Tianjin University, Tianjin 300072 (China); Gao, C. [School of Materials Science and Engineering, Tianjin University, Tianjin 300072 (China)

2007-05-16

Hydroxyapatite (HAp) and bacterial cellulose (BC) are both excellent materials for use in biomaterial areas. The former has outstanding osteoconductivity and bioactivity and the latter is a high-strength nano-fibrous and extensively used biomaterial. In this work, the HAp/BC nanocomposites with a 3-dimensional (3-D) network were synthesized via a biological route by soaking both phosphorylated and unphosphorylated BCs in 1.5 simulated body fluid (SBF). Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), and transmission electron microscopy (TEM) were employed to characterize the HAp/BC nanocomposites. SEM observations demonstrated that HAp crystals were uniformly formed on the phosphorylated BC fibers after soaking in 1.5 SBF whereas little HAp was observed on individual unphosphorylated BC fibers. Our experimental results suggested that the unphosphorylated BC did not induce HAp growth and that phosphorylation effectively triggered HAp formation on BC. Mechanisms were proposed for the explanation of the experimental observations. XRD and FTIR results revealed that the HAp crystals formed on the phosphorylated BC fibers were carbonate-containing with nano-sized crystallites and crystallinities less than 1%. These structural features were close to those of biological apatites.

Facile green synthesis of silver doped fluor-hydroxyapatite/β-cyclodextrin nanocomposite in the dual acting fluorine-containing ionic liquid medium for bone substitute applications

Energy Technology Data Exchange (ETDEWEB)

Jegatheeswaran, S. [Advanced Green Chemistry Lab, Department of Industrial Chemistry, School of Chemical Sciences, Alagappa University, Karaikudi-3, Tamil Nadu (India); Selvam, S. [Laser and Sensor Application Laboratory, Pusan National University, Busan 609735 (Korea, Republic of); Sri Ramkumar, V. [Deptartment of Environmental Biotechnology, School of Environmental, Sciences, Bharathidasan University, Tiruchirappalli, Tamilnadu (India); Sundrarajan, M., E-mail: sundrarajan@yahoo.com [Advanced Green Chemistry Lab, Department of Industrial Chemistry, School of Chemical Sciences, Alagappa University, Karaikudi-3, Tamil Nadu (India)

2016-05-15

Highlights: • Fluorine based ionic liquid was highly influenced the morphological structure of nanocomposites. • These composites has been motivated controlled release of silver nanoparticles for uniform antibacterial activity. • These material has given excellent antibacterial biofilm activity and favourable cytotoxical behavior on the human osteosarcoma (MG-63) cells. • These material has been highly suitable for bone substitute appliactions. - Abstract: A novel green route has approached for the synthesis of silver doped fluor-hydroxyapatite/β-cyclodextrin composite by the assistance of fluorine-based ionic liquid. The selected [BMIM]BF{sub 4} ionic liquid for this work plays a dual role as fluoride source and templating agent. It helps to improve the crystalline structures and the shape of the composites. The crystallinity, surface morphology, topographical studies of the synthesized composite were validated. The XRD results of the composite show typical Ag reflection peaks at 38.1°, 44.2° and 63.4°. The ionic liquid assisted composite displayed the hexagonal shaped HA particles, which are surrounded by spherical nano-Ag particles and these particles are uniformly dispersed in the β-cyclodextrin matrix in both horizontal and cross sections from surface morphology observations. The Ionic liquid assisted silver doped fluor-hydroxyapatite/β-cyclodextrin composite exhibited very good antibacterial activities against Escherichia coli, Salmonella typhi, Klebsiella pneumonia and Serratia liquefaciens pathogens. The antibacterial proficiencies were established using Confocal Laser Scanning Microscopic developed biofilms images and bacterial growth curve analysis. The cytotoxicity results of the ionic liquid assisted composite analyzed by cell proliferation in vitro studies using human osteosarcoma cell line (MG-63) and this study has shown excellent biocompatibility.

Facile green synthesis of silver doped fluor-hydroxyapatite/β-cyclodextrin nanocomposite in the dual acting fluorine-containing ionic liquid medium for bone substitute applications

International Nuclear Information System (INIS)

Jegatheeswaran, S.; Selvam, S.; Sri Ramkumar, V.; Sundrarajan, M.

2016-01-01

Highlights: • Fluorine based ionic liquid was highly influenced the morphological structure of nanocomposites. • These composites has been motivated controlled release of silver nanoparticles for uniform antibacterial activity. • These material has given excellent antibacterial biofilm activity and favourable cytotoxical behavior on the human osteosarcoma (MG-63) cells. • These material has been highly suitable for bone substitute appliactions. - Abstract: A novel green route has approached for the synthesis of silver doped fluor-hydroxyapatite/β-cyclodextrin composite by the assistance of fluorine-based ionic liquid. The selected [BMIM]BF_4 ionic liquid for this work plays a dual role as fluoride source and templating agent. It helps to improve the crystalline structures and the shape of the composites. The crystallinity, surface morphology, topographical studies of the synthesized composite were validated. The XRD results of the composite show typical Ag reflection peaks at 38.1°, 44.2° and 63.4°. The ionic liquid assisted composite displayed the hexagonal shaped HA particles, which are surrounded by spherical nano-Ag particles and these particles are uniformly dispersed in the β-cyclodextrin matrix in both horizontal and cross sections from surface morphology observations. The Ionic liquid assisted silver doped fluor-hydroxyapatite/β-cyclodextrin composite exhibited very good antibacterial activities against Escherichia coli, Salmonella typhi, Klebsiella pneumonia and Serratia liquefaciens pathogens. The antibacterial proficiencies were established using Confocal Laser Scanning Microscopic developed biofilms images and bacterial growth curve analysis. The cytotoxicity results of the ionic liquid assisted composite analyzed by cell proliferation in vitro studies using human osteosarcoma cell line (MG-63) and this study has shown excellent biocompatibility.

The TL and OSL study of hydroxyapatites for dosimetric applications

International Nuclear Information System (INIS)

Alencar, Marcus A. Vallim de

2009-01-01

The hydroxyapatite, the principal mineral component of the bone and tooth enamel, is one of the dosimetric materials that has distinguished itself in the high dose and accidents dosimetry, as well as in the dating, for the Electron Paramagnetic Resonance (EPR) technique. For this reason, the hydroxyapatite could also be used as Thermoluminescence (TL) and Optically Stimulated Luminescence (OSL) dosimeter in the dosimetry of high doses and accidents, and also in the archaeological and geological dating. This work presents a brief study of the TL and OSL behaviour of the B type synthetic carbonated hydroxyapatite, observing the possibility to use this material in TL and OSL dosimetry. The samples were irradiated to a dose of 100 Gy and 1000 Gy, and the TL and OSL measurements were obtained by the RISOE TL/OSL reader, model TL/OSL-DA-15B. The first results demonstrate the presence of three peaks in the TL glow curve in the temperatures of 100 deg C, 150 deg C and 280 deg C. The synthetic carbonated hydroxyapatite also presents an OSL signal when the sample is stimulated with blue light and a small OSL signal for stimulation with infrared light (IR). These results indicate the possibility of this synthetic carbonated hydroxyapatite to be used as dose indicator material using the TL and OSL techniques. (author)

Bisphosphonates enhance bacterial adhesion and biofilm formation on bone hydroxyapatite.

Science.gov (United States)

Kos, Marcin; Junka, Adam; Smutnicka, Danuta; Szymczyk, Patrycja; Gluza, Karolina; Bartoszewicz, Marzenna

2015-07-01

Because of the suspicion that bisphosphonates enhance bacterial colonization, this study evaluated adhesion and biofilm formation by Streptococcus mutans 25175, Staphylococcus aureus 6538, and Pseudomonas aeruginosa 14454 reference strains on hydroxyapatite coated with clodronate, pamidronate, or zoledronate. Bacterial strains were cultured on bisphosphonate-coated and noncoated hydroxyapatite discs. After incubation, nonadhered bacteria were removed by centrifugation. Biofilm formation was confirmed by scanning electron microscopy. Bacterial colonization was estimated using quantitative cultures compared by means with Kruskal-Wallis and post-hoc Student-Newman-Keuls tests. Modeling of the interactions between bisphosphonates and hydroxyapatite was performed using the Density Functional Theory method. Bacterial colonization of the hydroxyapatite discs was significantly higher for all tested strains in the presence of bisphosphonates vs. Adherence in the presence of pamidronate was higher than with other bisphosphonates. Density Functional Theory analysis showed that the protonated amine group of pamidronate, which are not present in clodronate or zoledronate, forms two additional hydrogen bonds with hydroxyapatite. Moreover, the reactive cationic amino group of pamidronate may attract bacteria by direct electrostatic interaction. Increased bacterial adhesion and biofilm formation can promote osteomyelitis, cause failure of dental implants or bisphosphonate-coated joint prostheses, and complicate bone surgery in patients on bisphosphonates. Copyright © 2015 European Association for Cranio-Maxillo-Facial Surgery. Published by Elsevier Ltd. All rights reserved.

In vitro mechanical integrity of hydroxyapatite coated magnesium alloy.

Science.gov (United States)

Kannan, M Bobby; Orr, Lynnley

2011-08-01

The mechanical integrity of resorbable implants during service, especially in load bearing orthopaedic applications, is critical. The high degradation rate of resorbable magnesium and magnesium-based implants in body fluid may potentially cause premature in-service failure. In this study, a magnesium alloy (AZ91) was potentiostatically coated with hydroxyapatite at different cathodic voltages in an attempt to enhance the mechanical integrity. The mechanical integrity of the uncoated and hydroxyapatite coated alloys was evaluated after in vitro testing of the coated samples in simulated body fluid (SBF). The uncoated alloy showed 40% loss in the mechanical strength after five days exposure to SBF. However, the hydroxyapatite coated alloy exposed to SBF showed 20% improvement in the mechanical strength as compared to that of the uncoated alloy. The alloy coated potentiostatically at -2 V performed better than the -3 V coated alloy. The cross-sectional analysis of the coatings revealed relatively uniform coating thickness for the -2 V coated alloy, whereas the -3 V coated alloy exhibited areas of uneven coating. This can be attributed to the increase in hydrogen evolution on the alloy during -3 V coating as compared to -2 V coating. The scanning electron micrographs of the in vitro tested alloy revealed that hydroxyapatite coating significantly reduced the localized corrosion of the alloy, which is critical for better in-service mechanical integrity. Thus, the study suggests that the in vitro mechanical integrity of resorbable magnesium-based alloy can be improved by potentiostatic hydroxyapatite coating. © 2011 IOP Publishing Ltd

Application of x-ray nano-particulate markers for the visualization of intermediate layers and interfaces using scanning electron microscopy

Science.gov (United States)

Bessudnova, Nadezda O.; Bilenko, David I.; Zakharevich, Andrey M.

2012-03-01

In this study the methodology of biological sample preparation for dental research using SEM/EDX has been elaborated. (1)The original cutting equipment supplied with 3D user-controlled sample fixation and an adjustable cooling system has been designed and evaluated. (2) A new approach to the root dentine drying procedure has been developed to preserve structure peculiarities of root dentine. (3) A novel adhesive system with embedded X-Ray nanoparticulate markers has been designed. (4)The technique allowing for visualization of bonding resins, interfaces and intermediate layers between tooth hard tissues and restorative materials of endodontically treated teeth using the X-ray nano-particulate markers has been developed and approved. These methods and approaches were used to compare the objective depth of penetration of adhesive systems of different generations in root dentine. It has been shown that the depth of penetration in dentine is less for adhesive systems of generation VI in comparison with bonding resins of generation V, which is in agreement with theoretical evidence. The depth of penetration depends on the correlation between the direction of dentinal tubules, bonding resin delivery and gravity.

Cerium doped hydroxyapatite nanoparticles synthesized by coprecipitation method

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Ciobanu Carmen Steluta

2016-01-01

Full Text Available The present work reports a simple coprecipitation adapted method for the synthesis of stable Ce substituted to Ca hydroxyapatite (HAp nanoparticles. The structural and morphological properties of Ce doped hydroxyapatite (Ce:HAp were characterized by X-ray diffraction (XRD, Transmission Electron Microscopy (TEM, Scanning Electron Microscopy (SEM and Energy Dispersive X-ray analysis (EDAX. The optical properties of Ce doped hydroxyapatite were also investigated using Fourier Transform Infrared (FTIR spectroscopy, FT Raman spectroscopy and photoluminescence analysis. The results of the XRD studies revealed the progressive increase in the a- and c-axes with increasing of Ce concentrations. In the FTIR studies of Ce:HAp powders a similar structure to hydroxyapatite was observed. IR and Raman wavenumbers and the peak strength of the bands associated to the P-O and O-H bonds decreases progressively with the increase of Ce concentration. All the emission maxima could be attributed to the 5d-4f transitions of Ce ions. The displacement of maximum emission bands with the increase of Cerium in the samples is in agreement with the results obtained by XRD studies. The Ce:HAp samples with xCe =0.03 and 0.05 exhibited significant antibacterial activity against Staphylococcus aureus ATCC 6538 and E. coli 714 bacterial strains compared to Ce:HAp samples with xCe =0 (pure HAp and 0.01.

Evolving application of biomimetic nanostructured hydroxyapatite

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Norberto Roveri

2010-11-01

Full Text Available Norberto Roveri, Michele IafiscoLaboratory of Environmental and Biological Structural Chemistry (LEBSC, Dipartimento di Chimica ‘G. Ciamician’, Alma Mater Studiorum, Università di Bologna, Bologna, ItalyAbstract: By mimicking Nature, we can design and synthesize inorganic smart materials that are reactive to biological tissues. These smart materials can be utilized to design innovative third-generation biomaterials, which are able to not only optimize their interaction with biological tissues and environment, but also mimic biogenic materials in their functionalities. The biomedical applications involve increasing the biomimetic levels from chemical composition, structural organization, morphology, mechanical behavior, nanostructure, and bulk and surface chemical–physical properties until the surface becomes bioreactive and stimulates cellular materials. The chemical–physical characteristics of biogenic hydroxyapatites from bone and tooth have been described, in order to point out the elective sides, which are important to reproduce the design of a new biomimetic synthetic hydroxyapatite. This review outlines the evolving applications of biomimetic synthetic calcium phosphates, details the main characteristics of bone and tooth, where the calcium phosphates are present, and discusses the chemical–physical characteristics of biomimetic calcium phosphates, methods of synthesizing them, and some of their biomedical applications.Keywords: hydroxyapatite, nanocrystals, biomimetism, biomaterials, drug delivery, remineralization

XRD and SEM analysis of hydroxyapatite during immersion in stimulated physiological solutions

International Nuclear Information System (INIS)

Yusof Abdullah; Idris Besar; Rosmamuhamadani Ramli; Abd Razak Daud

2000-01-01

XRD and SEM techniques were used to analyse the apatite layer developed on the synthetic hydroxyapatite surface following immersion in the simulated body fluid (SBF) that mimics the conditions of material experiences after implantation in the human body. Initially, the new layers formed after 7 day's incubation and increased with immersion time as crystallization of apatite phase. The XRD confirmed that the deposited layer was hydroxyapatite and crystallographically. With time, the crystal growth become more random and the intensity of the peaks decreased. During immersion, hydroxyapatite was precipitated from the SBF and coherently scattered with very small crystal. The SEM observation shows that the new precipitates were increased as well as incubation period increased. Therefore, hydroxyapatite ceramics are suggested to have very good biocompatibility. (Author)

Hydroxyapatite/poly(epsilon-caprolactone) double coating on magnesium for enhanced corrosion resistance and coating flexibility.

Science.gov (United States)

Jo, Ji-Hoon; Li, Yuanlong; Kim, Sae-Mi; Kim, Hyoun-Ee; Koh, Young-Hag

2013-11-01

Hydroxyapatite was deposited on pure magnesium (Mg) with a flexible poly(ε-caprolactone) interlayer to reduce the corrosion rate of Mg and enhance coating flexibility. The poly(ε-caprolactone) interlayer was uniformly coated on Mg by a spraying method, followed by hydroxyapatite deposition on the poly(ε-caprolactone) using an aerosol deposition method. In scanning electron microscopy observations, inorganic/organic composite-like structure was observed between the hydroxyapatite and poly(ε-caprolactone) layers, resulting from the collisions of hydroxyapatite particles into the poly(ε-caprolactone) matrix at the initial stage of the aerosol deposition. The corrosion resistance of the coated Mg was examined using potentiodynamic polarization tests. The hydroxyapatite/poly(ε-caprolactone) double coating remarkably improved the corrosion resistance of Mg in Hank's solution. In the in vitro cell tests, the coated Mg showed better cell adhesion compared with the bare Mg due to the reduced corrosion rate and enhanced biocompatibility. The stability and flexibility of hydroxyapatite/poly(ε-caprolactone) double coating was investigated by scanning electron microscopy inspections after the coated Mg was deformed. The hydroxyapatite coating on the poly(ε-caprolactone) interlayer revealed enhanced coating stability and flexibility without cracking or delamination during bending and stretching compared with the hydroxyapatite single coating. These results demonstrated that the hydroxyapatite/poly(ε-caprolactone) double coating significantly improved the surface corrosion resistance of Mg and enhanced coating flexibility for use of Mg as a biodegradable implant.

Influence of Starting Powders on Hydroxyapatite Coatings Fabricated by Room Temperature Spraying Method.

Science.gov (United States)

Seo, Dong Seok; Lee, Jong Kook; Hwang, Kyu Hong; Hahn, Byung Dong; Yoon, Seog Young

2015-08-01

Three types of raw materials were used for the fabrication of hydroxyapatite coatings by using the room temperature spraying method and their influence on the microstructure and in vitro characteristics were investigated. Starting hydroxyapatite powders for coatings on titanium substrate were prepared by a heat treatment at 1100 °C for 2 h of bovine bone, bone ash, and commercial hydroxyapatite powders. The phase compositions and Ca/P ratios of the three hydroxyapatite coatings were similar to those of the raw materials without decomposition or formation of a new phase. All hydroxyapatite coatings showed a honeycomb structure, but their surface microstructures revealed different features in regards to surface morphology and roughness, based on the staring materials. All coatings consisted of nano-sized grains and had dense microstructure. Inferred from in vitro experiments in pure water, all coatings have a good dissolution-resistance and biostability in water.

Converted marine coral hydroxyapatite implants with growth factors: In vivo bone regeneration

Energy Technology Data Exchange (ETDEWEB)

Nandi, Samit K., E-mail: samitnandi1967@gmail.com [Department of Veterinary Surgery and Radiology, West Bengal University of Animal and Fishery Sciences, Kolkata (India); Kundu, Biswanath, E-mail: biswa_kundu@rediffmail.com [Bioceramics and Coating Division, CSIR-Central Glass and Ceramic Research Institute, Kolkata (India); Mukherjee, Jayanta [Institute of Animal Health and Veterinary Biologicals, Kolkata (India); Mahato, Arnab; Datta, Someswar; Balla, Vamsi Krishna [Bioceramics and Coating Division, CSIR-Central Glass and Ceramic Research Institute, Kolkata (India)

2015-04-01

Herein we report rabbit model in vivo bone regeneration of hydrothermally converted coralline hydroxyapatite (HCCHAp) scaffolds without (group I) and with growth factors namely insulin like growth factor-1 (IGF-1) (group II) and bone morphogenetic protein-2 (BMP-2) (group III). All HCCHAp scaffolds have been characterized for phase purity and morphology before implantation. Calcined marine coral was hydrothermally converted using a mineralizer/catalyst to phase pure HAp retaining original pore structure and geometry. After sintering at 1250 °C, the HCCHAp found to have ~ 87% crystallinity, 70–75% porosity and 2 ± 0.5 MPa compressive strength. In vitro growth factor release study at day 28 revealed 77 and 98% release for IGF-1 and BMP-2, respectively. The IGF-1 release was more sustained than BMP-2. In vivo bone healing of different groups was compared using chronological radiology, histological evaluations, scanning electron microscopy and fluorochrome labeling up to 90 days of implantation. In vivo studies showed substantial reduction in radiolucent zone and decreased radiodensity of implants in group II followed by group III and group I. These observations clearly suggest in-growth of osseous tissue, initiation of bone healing and complete union between implants and natural bone in group II implants. A statistical score sheet based on histological observations showed an excellent osseous tissue formation in group II and group III scaffolds and moderate bone regeneration in group I scaffolds. - Highlights: • In vivo bone regeneration of hydrothermally converted coralline hydroxyapatite • Scaffolds with and without growth factors (IGF-1 and BMP-2) • In vitro drug release was more sustained for IGF-1 than BMP-2. • Growth factor significantly improved osseous tissue formation of implanted scaffold. • Established through detailed statistical score sheet from histological observations.

Converted marine coral hydroxyapatite implants with growth factors: In vivo bone regeneration

International Nuclear Information System (INIS)

Nandi, Samit K.; Kundu, Biswanath; Mukherjee, Jayanta; Mahato, Arnab; Datta, Someswar; Balla, Vamsi Krishna

2015-01-01

Herein we report rabbit model in vivo bone regeneration of hydrothermally converted coralline hydroxyapatite (HCCHAp) scaffolds without (group I) and with growth factors namely insulin like growth factor-1 (IGF-1) (group II) and bone morphogenetic protein-2 (BMP-2) (group III). All HCCHAp scaffolds have been characterized for phase purity and morphology before implantation. Calcined marine coral was hydrothermally converted using a mineralizer/catalyst to phase pure HAp retaining original pore structure and geometry. After sintering at 1250 °C, the HCCHAp found to have ~ 87% crystallinity, 70–75% porosity and 2 ± 0.5 MPa compressive strength. In vitro growth factor release study at day 28 revealed 77 and 98% release for IGF-1 and BMP-2, respectively. The IGF-1 release was more sustained than BMP-2. In vivo bone healing of different groups was compared using chronological radiology, histological evaluations, scanning electron microscopy and fluorochrome labeling up to 90 days of implantation. In vivo studies showed substantial reduction in radiolucent zone and decreased radiodensity of implants in group II followed by group III and group I. These observations clearly suggest in-growth of osseous tissue, initiation of bone healing and complete union between implants and natural bone in group II implants. A statistical score sheet based on histological observations showed an excellent osseous tissue formation in group II and group III scaffolds and moderate bone regeneration in group I scaffolds. - Highlights: • In vivo bone regeneration of hydrothermally converted coralline hydroxyapatite • Scaffolds with and without growth factors (IGF-1 and BMP-2) • In vitro drug release was more sustained for IGF-1 than BMP-2. • Growth factor significantly improved osseous tissue formation of implanted scaffold. • Established through detailed statistical score sheet from histological observations

Nanocrystalline hydroxyapatite enriched in selenite and manganese ions: physicochemical and antibacterial properties

Science.gov (United States)

Kolmas, Joanna; Groszyk, Ewa; Piotrowska, Urszula

2015-07-01

In this work, we used the co-precipitation method to synthesize hydroxyapatite (Mn-SeO3-HA) containing both selenium IV (approximately 3.60 wt.%) and manganese II (approximately 0.29 wt.%). Pure hydroxyapatite (HA), hydroxyapatite-containing manganese (II) ions (Mn-HA), and hydroxyapatite-containing selenite ions alone (SeO3-HA), prepared with the same method, were used as reference materials. The structures and physicochemical properties of all the obtained samples were investigated. PXRD studies showed that the obtained materials were homogeneous and consisted of apatite phase. Introducing selenites into the hydroxyapatite crystals considerably affects the size and degree of ordering. Experiments with transmission electron microscopy (TEM) showed that Mn-SeO3-HA crystals are very small, needle-like, and tend to form agglomerates. Fourier transform infrared spectroscopy (FT-IR) and solid-state nuclear magnetic resonance (ssNMR) were used to analyze the structure of the obtained material. Preliminary microbiological tests showed that the material demonstrated antibacterial activity against Staphylococcus aureus, yet such properties were not confirmed regarding Escherichia coli. PACS codes: 61, 76, 81

Mechanical Properties of Chitosan-Starch Composite Filled Hydroxyapatite Micro- and Nanopowders

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Jafar Ai

2011-01-01

Full Text Available Hydroxyapatite is a biocompatible ceramic and reinforcing material for bone implantations. In this study, Starch-chitosan hydrogel was produced using the oxidation of starch solution and subsequently cross-linked with chitosan via reductive alkylation method (weight ratio (starch/chitosan: 0.38. The hydroxyapatite micropowders and nanopowders synthesized by sol-gel method (10, 20, 30, 40 %W were composited to hydrogels and were investigated by mechanical analysis. The results of SEM images and Zetasizer experiments for synthesized nanopowders showed an average size of 100 nm. The nanoparticles distributed as uniform in the chitosan-starch film. The tensile modulus increased for composites containing hydroxyapatite nano-(size particle: 100 nanometer powders than composites containing micro-(size particle: 100 micrometer powders. The swelling percentage decreased for samples containing hydroxyapatite nanopowder than the micropowders. These nanocomposites could be applied for hard-tissue engineering.

Crystalline Silica Primer

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,

1992-01-01

Crystalline silica is the scientific name for a group of minerals composed of silicon and oxygen. The term crystalline refers to the fact that the oxygen and silicon atoms are arranged in a threedimensional repeating pattern. This group of minerals has shaped human history since the beginning of civilization. From the sand used for making glass to the piezoelectric quartz crystals used in advanced communication systems, crystalline silica has been a part of our technological development. Crystalline silica's pervasiveness in our technology is matched only by its abundance in nature. It's found in samples from every geologic era and from every location around the globe. Scientists have known for decades that prolonged and excessive exposure to crystalline silica dust in mining environments can cause silicosis, a noncancerous lung disease. During the 1980's, studies were conducted that suggested that crystalline silica also was a carcinogen. As a result of these findings, crystalline silica has been regulated under the Occupational Safety and Health Administration's (OSHA) Hazard Communication Standard (HCS). Under HCS, OSHAregulated businesses that use materials containing 0.1% or more crystalline silica must follow Federal guidelines concerning hazard communication and worker training. Although the HCS does not require that samples be analyzed for crystalline silica, mineral suppliers or OSHAregulated

Mechanical characterisation of porous glass reinforced hydroxyapatite ceramics: Bonelike®

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Marcelo Henrique Prado da Silva

2003-06-01

Full Text Available In the present study, mechanical properties of porous glass reinforced hydroxyapatite bioceramics were assessed by microhardness, bending and compression tests and fracture toughness determination. Porous discs were produced by a dry method using wax spheres as pore formers. Green bodies were sintered and the final microstructure of the composites consists of hydroxyapatite, alpha and beta tricalcium phosphate (alpha and b-Ca3(PO42due to the reaction between the glassy phase and the hydroxyapatite matrix. The results of the mechanical tests showed that the glassy phase yielded higher fracture toughness and bending strength when comparing with literature data for single hydroxyapatite. There is a compromise between mechanical properties and the porosity level for bioceramics: for example, according to Weibull statistics for composites with 65% porosity the maximum bending stress level is 0.2 MPa for 100% survival probability whereas this stress level increases to 2.5 MPa for composites with 40%. However, only the 65% porosity composite samples seem to have the complete adequate morphology for bone ingrowth.

FORMATION OF CHLOROPYROMORPHITE IN A LEAD-CONTAMINATED SOIL AMENDED WITH HYDROXYAPATITE

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To evaluate conversion of soil Pb to pyromorphite, a Pb contaminated soil collected adjacent to a historical smelter was reacted with hydroxyapatite in a traditional incubation experiment and in a dialysis system in which the soil and hydroxyapatite solids were separated by a dia...

Synthesis of hydroxyapatite coatings on metal substrates using a spincasting technique

International Nuclear Information System (INIS)

Yuan Qiuhua; Sahu, Laxmi Kumari; D'Souza, Nandika A.; Golden, Teresa Diane

2009-01-01

Hydroxyapatite coatings on stainless steel substrates were prepared by a simple spincasting technique. Nanosized hydroxyapatite powders were prepared by precipitating in an electrolytic suspension, and then added to a polylactic acid solution for spincasting. The polylactic acid gave enhanced protection from corrosion and inhibited decomposition of the hydroxyapatite coating during the sintering process in air, a significant advantage over other solution processing techniques. Characterization of the phase composition and morphology of the fabricated films on stainless steel was accomplished by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy.

Development of Antibiotics Impregnated Nanosized Silver Phosphate-Doped Hydroxyapatite Bone Graft

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Waraporn Suvannapruk

2013-01-01

Full Text Available Nanosized Ag3PO4 loaded hydroxyapatite which was prepared by a novel low temperature phosphorization of 3D printed calcium sulfate dihydrate at the nominal silver concentration of 0.001 M and 0.005 M was impregnated by two antibiotics including gentamicin and vancomycin. Phase composition, microstructure, antibiotics loading, silver content, antimicrobial performance, and cytotoxic potential of the prepared samples were characterized. It was found that the fabricated sample consisted of hydroxyapatite as a main phase and spherical-shaped silver phosphate nanoparticles distributing within the cluster of hydroxyapatite crystals. Antibacterial activity of the samples against two bacterial strains (gram negative P. aeruginosa and gram positive S. aureus was carried out. It was found that the combination of antibiotics and nanosized Ag3PO4 in hydroxyapatite could enhance the antibacterial performance of the samples by increasing the duration in which the materials exhibited antibacterial property and the size of the inhibition zone depending on the type of antibiotics and bacterial strains compared to those contained antibiotics or nanosilver phosphate alone. Cytotoxic potential against osteoblasts of antibiotics impregnated nanosilver phosphate hydroxyapatite was found to depend on the combination of antibiotics content, type of antibiotics, and nanosilver phosphate content.

Fabrication and Microstructure of Hydroxyapatite Coatings on Zirconia by Room Temperature Spray Process.

Science.gov (United States)

Seo, Dong Seok; Chae, Hak Cheol; Lee, Jong Kook

2015-08-01

Hydroxyapatite coatings were fabricated on zirconia substrates by a room temperature spray process and were investigated with regards to their microstructure, composition and dissolution in water. An initial hydroxyapatite powder was prepared by heat treatment of bovine-bone derived powder at 1100 °C for 2 h, while dense zirconia substrates were fabricated by pressing 3Y-TZP powder and sintering it at 1350 °C for 2 h. Room temperature spray coating was performed using a slit nozzle in a low pressure-chamber with a controlled coating time. The phase composition of the resultant hydroxyapatite coatings was similar to that of the starting powder, however, the grain size of the hydroxyapatite particles was reduced to about 100 nm due to their formation by particle impaction and fracture. All areas of the coating had a similar morphology, consisting of reticulated structure with a high surface roughness. The hydroxyapatite coating layer exhibited biostability in a stimulated body fluid, with no severe dissolution being observed during in vitro experimentation.

Titanium-hydroxyapatite composites sintered at low temperature for tissue engineering: in vitro cell support and biocompatibility.

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Comín, Romina; Cid, Mariana P; Grinschpun, Luciano; Oldani, Carlos; Salvatierra, Nancy A

2017-04-26

In clinical orthopedics, a critical problem is the bone tissue loss produced by a disease or injury. The use of composites from titanium and hydroxyapatite for biomedical applications has increased due to the resulting advantageous combination of hydroxyapatite bioactivity and favorable mechanical properties of titanium. Powder metallurgy is a simple and lower-cost method that uses powder from titanium and hydroxyapatite to obtain composites having hydroxyapatite phases in a metallic matrix. However, this method has certain limitations arising from thermal decomposition of hydroxyapatite in the titanium-hydroxyapatite system above 800°C. We obtained a composite from titanium and bovine hydroxyapatite powders sintered at 800°C and evaluated its bioactivity and cytocompatibility according to the ISO 10993 standard. Surface analysis and bioactivity of the composite was evaluated by X-ray diffraction and SEM. MTT assay was carried out to assess cytotoxicity on Vero and NIH3T3 cells. Cell morphology and cell adhesion on the composite surface were analyzed using fluorescence and SEM. We obtained a porous composite with hydroxyapatite particles well integrated in titanium matrix which presented excellent bioactivity. Our data did not reveal any toxicity of titanium-hydroxyapatite composite on Vero or NIH3T3 cells. Moreover, extracts from composite did not affect cell morphology or density. Finally, NIH3T3 cells were capable of adhering to and proliferating on the composite surface. The composite obtained displayed promising biomedical applications through the simple method of powder metallurgy. Additionally, these findings provide an in vitro proof for adequate biocompatibility of titanium-hydroxyapatite composite sintered at 800°C.

Preparation of hydroxyapatite nanoparticles facilitated by the presence of {beta}-cyclodextrin

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Martinez-Perez, Carlos A., E-mail: camartin@uacj.mx [Institute of Engineering and Technology, Autonomous University of Juarez, UACJ, Ave. del Charro 610 norte, C.P. 32320, Cd. Juarez, Chihuahua (Mexico); Garcia-Montelongo, Jorge; Garcia Casillas, Perla E.; Farias-Mancilla, Jose R. [Institute of Engineering and Technology, Autonomous University of Juarez, UACJ, Ave. del Charro 610 norte, C.P. 32320, Cd. Juarez, Chihuahua (Mexico); Monreal Romero, Humberto [School of Odontology, Autonomous University of Chihuahua, UACH, Ave. Universidad s/n Campus Universitario I, C.P. 31170, Chihuahua (Mexico)

2012-09-25

Highlights: Black-Right-Pointing-Pointer It was found that {beta}-cyclodextrin can control the particle size in the production of nanohydroxyapatite. Black-Right-Pointing-Pointer Particle size in the range of 30-50 nm was obtained. Black-Right-Pointing-Pointer A new simple methodology for the preparation of hydroxyapatite nanoparticles with a well controlled size and narrow particles size distribution was developed. - Abstract: Hydroxyapatite nanoparticles with uniform morphology have been successfully synthesized by a chemical coprecipitation method and facilitated by the presence of the {beta}-cyclodextrin. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM); and Fourier Transformed Infrared Spectroscopy (FT-IR) were used in order to characterize the hydroxyapatite samples. The experimental results indicate that the obtained HA is in the range of 20-50 nm. Also it was found that the content of {beta}-CD has an impact on the purity of the HA as well in the particle size of the hydroxyapatite nanoparticles.

Preparation of hydroxyapatite nanoparticles facilitated by the presence of β-cyclodextrin

International Nuclear Information System (INIS)

Martínez-Pérez, Carlos A.; García-Montelongo, Jorge; Garcia Casillas, Perla E.; Farias-Mancilla, José R.; Monreal Romero, Humberto

2012-01-01

Highlights: ► It was found that β-cyclodextrin can control the particle size in the production of nanohydroxyapatite. ► Particle size in the range of 30–50 nm was obtained. ► A new simple methodology for the preparation of hydroxyapatite nanoparticles with a well controlled size and narrow particles size distribution was developed. - Abstract: Hydroxyapatite nanoparticles with uniform morphology have been successfully synthesized by a chemical coprecipitation method and facilitated by the presence of the β-cyclodextrin. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM); and Fourier Transformed Infrared Spectroscopy (FT-IR) were used in order to characterize the hydroxyapatite samples. The experimental results indicate that the obtained HA is in the range of 20–50 nm. Also it was found that the content of β-CD has an impact on the purity of the HA as well in the particle size of the hydroxyapatite nanoparticles.

[Study on the antibacterial activity of four kinds of nano-hydroxyapatite composites against Enterococcus faecalis].

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Liu, Yi; Zhou, Rongjing; Wu, Hongkun

2015-06-01

This study aims to compare and determine a kind of nano-hydroxyapatite composite material with good antibacterial efficacy on Enterococcusfaecalis (E. faecalis) in vitro. We investigated the antimicrobial activity of four kinds of nano-hydroxyapatite composites, namely, silver/hydroxyapatite composite nanoparticles (Ag/nHA), yttrium/hydroxyapatite composite nanoparticles (Yi/nHA), cerium/hydroxyapatite composite nanoparticles (Ce/nHA), and hydroxyapatite nanoparticles (nHA), against E. faecalis in vitro using the agar diffusion and broth dilution method by measuring the growth inhibition zone and the minimum inhibitory concentration (MIC), respectively. The agar diffusion test results showed that Ag/nHA displayed an obvious growth inhibition zone, whereas Yi/nHA, Ce/nHA, and nHA showed no influence on E. faecalis. The MIC value of Ag/nHA was 1.0 g.L-1, and the three other materials had no effect on E.faecalis even at the high concentration of 32.0 g.L-1. Ag/nHA display a potential antimicrobial efficacy to planktonic E.faecalis. Whereas, the three other kinds of nano-hydroxyapatite composites (Yi/nHA, Ce/nHA, nHA) show no influence.

Sorption of fission nuclides on model milk components. I. Sorption of radiostrontium on hydroxyapatite in aqueous solutions

International Nuclear Information System (INIS)

Rosskopfova, O.; Kopunec, R.; Matel, L.; Macasek, F.; Kristin, J.

1999-01-01

Hydroxyapatite, Ca 10 (PO 4 ) 6 (OH) 2 is a mineral widely spread in nature as a main constituent of phosphate rocks, and also as the major inorganic component of bones and teeth. It was found that sorption process occurs by an ion exchange reaction mechanism between strontium ions in solution and calcium ions in apatite. Ca 2+ → Sr 2+ substitution in hydroxyapatite is important since it explains the mechanism of incorporation of beta-active Sr-90 of atomic debris into the human skeletal system. The strontium uptake at 100 grad C is done by adsorption and diffusion while at 25 grad C it is done by the process of adsorption only. The hydroxyapatite was prepared from aqueous solutions and characterized by standard analytical methods. Some samples of hydroxyapatite were modified by heating after its precipitation from aqueous solution. The sample obtained had characteristics of well crystallized stoichiometric hydroxyapatite. Also, commercial hydroxy-apatites were used. Sorption of strontium ions on synthetic hydroxyapatite was examined using batch method and sorption depends on the method of preparation of hydroxyapatite. In generally, sorption of strontium decreases with the increase in the particle size of hydroxyapatite and decreases with the increase in the pH ( hydroxyapatite surface is amphoteric and acts as a buffer in a wide pH range). The sorption of strontium increases with the increase in [Sr 2+ ] or [Ca 2+ ] in solution to ∼ 10 -5 mol · dm -3 for the hydroxyapatite prepared by heating. The experimental data for sorption of strontium has been fitted with Langmuir-adsorption isotherm. (authors)

Magnesium substitution in carbonated hydroxyapatite: Structural and microstructural characterization by Rietveld's refinement

Energy Technology Data Exchange (ETDEWEB)

Lala, S. [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India); Ghosh, M.; Das, P.K. [Department of Biological Chemistry, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700 032 (India); Das, D. [UGC-DAE Consortium for Scientific Research, Kolkata 700098 (India); Kar, T. [Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata 700032 (India); Pradhan, S.K., E-mail: skpradhan@phys.buruniv.ac.in [Materials Science Division, Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India)

2016-02-15

Four stoichiometric compositions of nanocrystalline Mg doped carbonated hydroxyapatite (cHAp) powders are synthesized by mechanical alloying (ball milling) the powder mixtures of CaCO{sub 3}, CaHPO{sub 4}.2H{sub 2}O and MgO in open air at room temperature. FTIR analysis confirms the A-type carbonation in all milled HAp powder samples (A-cHAp). Microstructure characterization in terms of lattice imperfections and phase quantification of ball milled samples are made by analyzing XRD patterns employing Rietveld's structure refinement method. Transmission electron microscopy (TEM) study of 15 mol % Mg doped A-cHAp sample reveals microstructure similar to that obtained from XRD pattern analysis. Cumulative effect of Mg substitution and mechanical alloying results in amorphization of a major part of crystalline A-cHAp, analogous to native bone mineral. Rietveld analysis reveals that the Ca2 vacancy site is energetically more favorable for occupation of Mg substitution. MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assay test reveals sufficiently high percentage cell viability confirming the cytocompatibility of the sample. - Graphical abstract: Mg substitution for Ca2 site. - Highlights: • Single phase Mg doped A-cHAp synthesized by mechanical alloying (MA). • FTIR analysis confirms A-type carbonation in HAp. • Amorphization of a part of crystalline A-cHAp due to MA and Mg insertion. • Mg{sup 2+} ions substitute the Ca2 vacancy site. • High cell viability under MTT assay.

Effect of Hydroxyapatite on Bone Integration in a Rabbit Tibial Defect Model

Science.gov (United States)

Sohn, Sung-Keun; Kim, Kyung-Taek; Kim, Chul-Hong; Ahn, Hee-Bae; Rho, Mee-Sook; Jeong, Min-Ho; Sun, Sang-Kyu

2010-01-01

Background The aim of the present study was to prepare hydroxyapatite (HA) and then characterize its effect on bone integration in a rabbit tibial defect model. The bone formation with different designs of HA was compared and the bony integration of several graft materials was investigated qualitatively by radiologic and histologic study. Methods Ten rabbits were included in this study; two holes were drilled bilaterally across the near cortex and the four holes in each rabbit were divided into four treatment groups (HAP, hydroxyapatite powder; HAC, hydroxyapatite cylinder; HA/TCP, hydroxyapatite/tri-calcium phosphate cylinder, and titanium cylinder). The volume of bone ingrowth and the change of bone mineral density were statistically calculated by computed tomography five times for each treatment group at 0, 2, 4, 6, and 8 weeks after grafting. Histologic analysis was performed at 8 weeks after grafting. Results The HAP group showed the most pronounced effect on the bone ingrowth surface area, which seen at 4, 6, and 8 weeks after graft (p 0.05). On histological examination, the HAP group revealed well-recovered cortical bone, but the bone was irregularly thickened and haphazardly admixed with powder. The HAC group showed similar histological features to those of the HA/TCP group; the cortical surface of the newly developed bone was smooth and the bone matrix on the surface of the cylinder was regularly arranged. Conclusions We concluded that both the hydroxyapatite powder and cylinder models investigated in our study may be suitable as a bone substitute in the rabbit tibial defect model, but their characteristic properties are quite different. In contrast to hydroxyapatite powder, which showed better results for the bone ingrowth surface, the hydroxyapatite cylinder showed better results for the sustained morphology. PMID:20514266

New nano-hydroxyapatite in bone defect regeneration: A histological study in rats.

Science.gov (United States)

Kubasiewicz-Ross, Paweł; Hadzik, Jakub; Seeliger, Julia; Kozak, Karol; Jurczyszyn, Kamil; Gerber, Hanna; Dominiak, Marzena; Kunert-Keil, Christiane

2017-09-01

Many types of bone substitute materials are available on the market. Researchers are refining new bone substitutes to make them comparable to autologous grafting materials in treatment of bone defects. The purpose of the study was to evaluate the osseoconductive potential and bone defect regeneration in rat calvaria bone defects treated with new synthetic nano-hydroxyapatite. The study was performed on 30 rats divided into 5 equal groups. New preproduction of experimental nano-hydroxyapatite material by NanoSynHap (Poznań, Poland) was tested and compared with commercially available materials. Five mm critical size defects were created and filled with the following bone grafting materials: 1) Geistlich Bio-Oss ® ; 2) nano-hydroxyapatite+β-TCP; 3) nano-hydroxyapatite; 4) nano-hydroxyapatite+collagen membrane. The last group served as controls without any augmentation. Bone samples from calvaria were harvested for histological and micro-ct evaluation after 8 weeks. New bone formation was observed in all groups. Histomorphometric analysis revealed an amount of regenerated bone between 34.2 and 44.4% in treated bone defects, whereas only 13.0% regenerated bone was found in controls. Interestingly, in group 3, no significant particles of the nano-HA material were found. In contrast, residual bone substitute material could be detected in all other test groups. Micro-CT study confirmed the results of the histological examinations. The new nano-hydroxyapatite provides comparable results to other grafts in the field of bone regeneration. Copyright © 2017 Elsevier GmbH. All rights reserved.

Elimination of radical on the x-ray irradiated hydroxyapatite compounds

International Nuclear Information System (INIS)

Ohta, M.; Yasuda, M.; Miyazawa, C.; Okamura, H.; Suzuki, Y.

2002-01-01

We investigate the elimination of radical produced in a human tooth and synthetic calcium-deficient hydroxyapatite compounds after X-ray irradiation. Used samples were enamel and dentine of a human tooth and synthetic calcium-deficient hydroxyapatite (DAp), and stoichiometric hydroxyapatite (HAp). The ESR signal intensities at nearly g = 2 in the samples after X-ray irradiation were proportional to the absorbed dose in the range from 6 to 39 Gy. And these ESR signal intensities of the samples soaked in various ion containing fluids decreased with soaking time. Especially, the decrease in these ESR signal intensities was remarkably large in the samples soaked in Na 2 HPO 4 aqueous solution. This fact suggests that the surface layer of the samples easily dissolves in ion containing fluids

Hydroxyapatite coatings deposited by liquid precursor plasma spraying: controlled dense and porous microstructures and osteoblastic cell responses

International Nuclear Information System (INIS)

Huang Yi; Song Lei; Liu Xiaoguang; Xiao Yanfeng; Wu Yao; Chen Jiyong; Wu Fang; Gu Zhongwei

2010-01-01

Hydroxyapatite coatings were deposited on Ti-6Al-4V substrates by a novel plasma spraying process, the liquid precursor plasma spraying (LPPS) process. X-ray diffraction results showed that the coatings obtained by the LPPS process were mainly composed of hydroxyapatite. The LPPS process also showed excellent control on the coating microstructure, and both nearly fully dense and highly porous hydroxyapatite coatings were obtained by simply adjusting the solid content of the hydroxyapatite liquid precursor. Scanning electron microscope observations indicated that the porous hydroxyapatite coatings had pore size in the range of 10-200 μm and an average porosity of 48.26 ± 0.10%. The osteoblastic cell responses to the dense and porous hydroxyapatite coatings were evaluated with human osteoblastic cell MG-63, in respect of the cell morphology, proliferation and differentiation, with the hydroxyapatite coatings deposited by the atmospheric plasma spraying (APS) process as control. The cell experiment results indicated that the heat-treated LPPS coatings with a porous structure showed the best cell proliferation and differentiation among all the hydroxyapatite coatings. Our results suggest that the LPPS process is a promising plasma spraying technique for fabricating hydroxyapatite coatings with a controllable microstructure, which has great potential in bone repair and replacement applications.

Size effect in X-ray and electron diffraction patterns from hydroxyapatite particles

International Nuclear Information System (INIS)

Suvorova, E.I.; Buffat, P.-A.

2001-01-01

High-resolution transmission electron microscopy (HRTEM), electron microdiffraction, and X-ray diffraction were used to study hydroxyapatite specimens with particle sizes from a few nanometers to several hundreds of nanometers. Diffuse scattering (without clear reflections in transmission diffraction patterns) or strongly broadened peaks in X-ray diffraction patterns are characteristic for agglomerated hydroxyapatite nanocrystals. However, HRTEM and microdiffraction showed that this cannot be considered as an indication of the amorphous state of the matter but rather as the demonstration of size effect and the morphological and structural features of hydroxyapatite nanocrystals

Processing and characterization of biocomposites Poly (3-hydroxybutyrate) / hydroxyapatite for temporary support in bone regeneration

International Nuclear Information System (INIS)

Cardoso, Cyntia Esteves; Ferreira, Willian Hermogenes; Andrade, Cristina Tristao

2011-01-01

Composite materials like biopolymer / hydroxyapatite (HA) has been attracting the interest of researchers because of its applications in medicine. These materials have been used as temporary supports during the regeneration of bone tissue. In this work, poly (3-hydroxybutyrate) (PHB) was chosen as matrix because it has good processability and biocompatibility. The HA was obtained by precipitation from calcium hydroxide and phosphoric acid, varying the speed of dripping, the synthesis temperature and time of calcination. The techniques of infrared absorption spectroscopy and X-ray diffraction (XRD) were used to characterize the samples synthesized HA. The biocomposites were prepared in an internal mixer, with compositions PHB / HA varied. After processing, the biocomposites were ground, characterized by XRD analysis and the crystallinity index. The aim of this study was to examine the variables during the synthesis of HA and its thermal treatment in order to obtain a powder of HA using a simple technique and accessible, creating good properties for the biocomposites prepared. (author)

Preparation and mechanical properties of photo-crosslinked poly(trimethylene carbonate) and nano-hydroxyapatite composites.

Science.gov (United States)

Geven, Mike A; Barbieri, Davide; Yuan, Huipin; de Bruijn, Joost D; Grijpma, Dirk W

2015-01-01

Composite materials of photo-crosslinked poly(trimethylene carbonate) and nanoscale hydroxyapatite were prepared and their mechanical characteristics for application as orbital floor implants were assessed. The composites were prepared by solvent casting poly(trimethylene carbonate) macromers with varying amounts of nano-hydroxyapatite and subsequent photo-crosslinking. The incorporation of the nano-hydroxyapatite into the composites was examined by thermogravimetric analysis, scanning electron microscopy and gel content measurements. The mechanical properties were investigated by tensile testing and trouser tearing experiments. Our results show that nano-hydroxyapatite particles can readily be incorporated into photo-crosslinked poly(trimethylene carbonate) networks. Compared to the networks without nano-hydroxyapatite, incorporation of 36.3 wt.% of the apatite resulted in an increase of the E modulus, yield strength and tensile strength from 2.2 MPa to 51 MPa, 0.5 to 1.4 N/mm2 and from 1.3 to 3.9 N/mm2, respectively. We found that composites containing 12.4 wt.% nano-hydroxyapatite had the highest values of strain at break, toughness and average tear propagation strength (376% , 777 N/mm2 and 3.1 N/mm2, respectively).

Geloina coaxans shell as calcium source on synthesis hydroxyapatite

Science.gov (United States)

Yanti, P. H.; Kamiah, A.

2018-04-01

Geloina coaxans shell (GCS) is one of mullusc shell mainly composed by calcium carbonate. In this work, calcium carbonate has been converted to calcium oxide by calcination at 1000°C for 12 hours. The calcined of geloina coaxans shell were treated with HNO3 to produce Ca(NO3)2 as calcium source on synthesis hydroxyapatite. Orthophosphoric acid (H3PO4) was used as phosphate donor. Reaction of Ca/P has been done by precipitation method at molar ratio of precursors of 1.67 and pH adjusted at 10 using NH4OH. The XRD result revealed that hydoxyapatite can be prepared at 3 M of HNO3 and stirring time for 240 minutes. Specific band of hydroxyapatite such as PO4 and OH observed using FTIR instrument. Analysis of crystal size using Schererr equation proved nanosize of powder hydroxyapatite can be produced.

Synthesis and antimicrobial activity of silver-doped hydroxyapatite nanoparticles.

Science.gov (United States)

Ciobanu, Carmen Steluta; Iconaru, Simona Liliana; Chifiriuc, Mariana Carmen; Costescu, Adrian; Le Coustumer, Philippe; Predoi, Daniela

2013-01-01

The synthesis of nanosized particles of Ag-doped hydroxyapatite with antibacterial properties is of great interest for the development of new biomedical applications. The aim of this study was the evaluation of Ca(10-x)Ag(x)(PO4)6(OH)2 nanoparticles (Ag:HAp-NPs) for their antibacterial and antifungal activity. Resistance to antimicrobial agents by pathogenic bacteria has emerged in the recent years and became a major health problem. Here, we report a method for synthesizing Ag doped nanocrystalline hydroxyapatite. A silver-doped nanocrystalline hydroxyapatite was synthesized at 100°C in deionised water. Also, in this paper Ag:HAp-NPs are evaluated for their antimicrobial activity against gram-positive and gram-negative bacteria and fungal strains. The specific antimicrobial activity revealed by the qualitative assay is demonstrating that our compounds are interacting differently with the microbial targets, probably due to the differences in the microbial wall structures.

Occurrence and behaviour of dissolved, nano-particulate and micro-particulate iron in waste waters and treatment systems: new insights from electrochemical analysis.

Science.gov (United States)

Matthies, R; Aplin, A C; Horrocks, B R; Mudashiru, L K

2012-04-01

Cyclic-, Differential Pulse- and Steady-state Microdisc Voltammetry (CV, DPV, SMV) techniques have been used to quantify the occurrence and fate of dissolved Fe(ii)/Fe(iii), nano-particulate and micro-particulate iron over a 12 month period in a series of net-acidic and net-alkaline coal mine drainages and passive treatment systems. Total iron in the mine waters is typically 10-100 mg L(-1), with values up to 2100 mg L(-1). Between 30 and 80% of the total iron occurs as solid phase, of which 20 to 80% is nano-particulate. Nano-particulate iron comprises 20 to 70% of the nominally "dissolved" (i.e. sedimentation are the only processes required to remove solid phase iron, these data have important implications for the generation or consumption of acidity during water treatment. In most waters, the majority of truly dissolved iron occurs as Fe(ii) (average 64 ± 22%). Activities of Fe(ii) do not correlate with pH and geochemical modelling shows that no Fe(ii) mineral is supersaturated. Removal of Fe(ii) must proceed via oxidation and hydrolysis. Except in waters with pH waters are generally supersaturated with respect to ferrihydrite and schwertmannite, and are not at redox equilibrium, indicating the key role of oxidation and hydrolysis kinetics on water treatment. Typically 70-100% of iron is retained in the treatment systems. Oxidation, hydrolysis, precipitation, coagulation and sedimentation occur in all treatment systems and - independent of water chemistry and the type of treatment system - hydroxides and oxyhydroxysulfates are the main iron sinks. The electrochemical data thus reveal the rationale for incomplete iron retention in individual systems and can thus inform future design criteria. The successful application of this low cost and rapid electrochemical method demonstrates its significant potential for real-time, on-site monitoring of iron-enriched waters and may in future substitute traditional analytical methods.

Galvanic deposition and characterization of brushite/hydroxyapatite coatings on 316L stainless steel

Energy Technology Data Exchange (ETDEWEB)

Blanda, Giuseppe [Laboratorio di Chimica Fisica Applicata, Dipartimento di Ingegneria Chimica Gestionale Informatica Meccanica, Università di Palermo, Viale delle Scienze, 90128 Palermo (Italy); Brucato, Valerio; Pavia, Francesco Carfì; Greco, Silvia [Dipartimento di Ingegneria Civile, Ambientale, Aerospaziale, dei Materiali, Università di Palermo, Viale delle Scienze, 90128 Palermo (Italy); Piazza, Salvatore; Sunseri, Carmelo [Laboratorio di Chimica Fisica Applicata, Dipartimento di Ingegneria Chimica Gestionale Informatica Meccanica, Università di Palermo, Viale delle Scienze, 90128 Palermo (Italy); Inguanta, Rosalinda, E-mail: rosalinda.inguanta@unipa.it [Laboratorio di Chimica Fisica Applicata, Dipartimento di Ingegneria Chimica Gestionale Informatica Meccanica, Università di Palermo, Viale delle Scienze, 90128 Palermo (Italy)

2016-07-01

In this work, brushite and brushite/hydroxyapatite (BS, CaHPO{sub 4}·H{sub 2}O; HA, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}) coatings were deposited on 316L stainless steel (316LSS) from a solution containing Ca(NO{sub 3}){sub 2}·4H{sub 2}O and NH{sub 4}H{sub 2}PO{sub 4} by a displacement reaction based on a galvanic contact, where zinc acts as sacrificial anode. Driving force for the cementation reaction arises from the difference in the electrochemical standard potentials of two different metallic materials (316LSS and Zn) immersed in an electrolyte, so forming a galvanic contact leading to the deposition of BS/HA on nobler metal. We found that temperature and deposition time affect coating features (morphology, structure, and composition). Deposits were characterized by means of several techniques. The morphology was investigated by scanning electron microscopy, the elemental composition was obtained by X-ray energy dispersive spectroscopy, whilst the structure was identified by Raman spectroscopy and X-ray diffraction. BS was deposited at all investigated temperatures covering the 316LSS surface. At low and moderate temperature, BS coatings were compact, uniform and with good crystalline degree. On BS layers, HA crystals were obtained at 50 °C for all deposition times, while at 25 °C, its presence was revealed only after long deposition time. Electrochemical studies show remarkable improvement in corrosion resistance. - Highlights: • Brushite/hydroxyapatite coatings were obtained by a galvanic deposition method. • Galvanic deposition is simple and cheap and does not require external power supply. • Temperature is a key parameter to control composition and morphology of coatings. • Ca/P ratio changes with deposition time, from about 1 up to an optimum value of 1.7. • Compact and adherent layer covering substrate surface were obtained on 316LSS.

Galvanic deposition and characterization of brushite/hydroxyapatite coatings on 316L stainless steel

International Nuclear Information System (INIS)

Blanda, Giuseppe; Brucato, Valerio; Pavia, Francesco Carfì; Greco, Silvia; Piazza, Salvatore; Sunseri, Carmelo; Inguanta, Rosalinda